CN114229885A - CdO/SnO2Composite nanocube gas-sensitive material, preparation method and application thereof in hydrogen detection - Google Patents
CdO/SnO2Composite nanocube gas-sensitive material, preparation method and application thereof in hydrogen detection Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 53
- 239000007789 gas Substances 0.000 title claims abstract description 51
- 239000001257 hydrogen Substances 0.000 title claims abstract description 37
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 37
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000001514 detection method Methods 0.000 title claims abstract description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 60
- 239000002131 composite material Substances 0.000 claims abstract description 34
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 20
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
- 239000012716 precipitator Substances 0.000 claims abstract description 10
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 10
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims abstract description 6
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims abstract description 6
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000005245 sintering Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000007795 chemical reaction product Substances 0.000 claims description 8
- 239000002243 precursor Substances 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 238000011084 recovery Methods 0.000 abstract description 8
- DZVRGWYMCGLNKJ-UHFFFAOYSA-J cadmium dichloride hemipentahydrate Chemical compound O.O.O.O.O.Cl[Cd]Cl.Cl[Cd]Cl DZVRGWYMCGLNKJ-UHFFFAOYSA-J 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 6
- 230000035945 sensitivity Effects 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 4
- 238000000975 co-precipitation Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 238000001308 synthesis method Methods 0.000 abstract 1
- 150000002431 hydrogen Chemical class 0.000 description 9
- 239000011734 sodium Substances 0.000 description 7
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- KHMOASUYFVRATF-UHFFFAOYSA-J tin(4+);tetrachloride;pentahydrate Chemical compound O.O.O.O.O.Cl[Sn](Cl)(Cl)Cl KHMOASUYFVRATF-UHFFFAOYSA-J 0.000 description 6
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 5
- 239000010931 gold Substances 0.000 description 5
- 229910052737 gold Inorganic materials 0.000 description 5
- 239000000919 ceramic Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910018487 Ni—Cr Inorganic materials 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 239000011540 sensing material Substances 0.000 description 2
- 230000005476 size effect Effects 0.000 description 2
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- -1 cadmium chloride (CdCl) pentahydrate Chemical class 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- WNBBZWPFBHTAGZ-UHFFFAOYSA-L dichlorocadmium pentahydrate Chemical compound O.O.O.O.O.Cl[Cd]Cl WNBBZWPFBHTAGZ-UHFFFAOYSA-L 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910000623 nickel–chromium alloy Inorganic materials 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G11/00—Compounds of cadmium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/02—Oxides
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
CdO/SnO2A composite nanocube gas-sensitive material, a preparation method and application thereof in hydrogen detection belong to the technical field of gas-sensitive materials. The invention takes stannic chloride hydrate and cadmium dichloride hydrate as raw materials, takes sodium hydroxide and sodium carbonate mixed solution as a precipitator, and adopts a coprecipitation synthesis method to prepare a series of CdO/SnO with different molar ratios2A composite nanocube gas sensitive material. Wherein, the molar ratio of the CdO to the SnO is 1:12The gas sensor made of the composite nanocube gas-sensitive material shows excellent hydrogen detection performance. At a lower working temperature (220 ℃), the hydrogen response has the advantages of high sensitivity, high selectivity, extremely short response-recovery time and the like, and the hydrogen response is very beneficial to the early stage of hydrogen leakageAnd (6) early warning. The preparation method of the gas-sensitive material has the advantages of simple preparation conditions, short synthesis period, low raw material cost and easy realization of large-scale production.
Description
Technical Field
The invention belongs to the technical field of gas-sensitive materials, and particularly relates to CdO/SnO2A composite nanocube gas-sensitive material, a preparation method and application thereof in hydrogen detection.
Background
As a clean energy carrier, hydrogen is widely used in industries such as hydrogen fuel cells, new energy automobiles, petrochemical industry, metallurgical industry, aerospace, food processing, electronics and the like. The rapid development of green hydrogen energy sources also contributes to the accelerated achievement of "carbon peaking", "carbon neutralization". However, the hydrogen is colorless and odorless and cannot be easily perceived by people, the lower explosion limit of the hydrogen in the air is only 4%, and the hydrogen can be ignited only by energy of less than 0.02 millijoule. This means that once hydrogen leaks, there is a high possibility of serious safety accidents. However, since the hydrogen molecule has a small size, there is a possibility of leakage in each stage of preparation, storage, transportation and use of hydrogen, and therefore, the development of a hydrogen sensor with high sensitivity, low detection limit and fast response-recovery is of great significance for early warning of hydrogen leakage.
SnO2The material is one of the classical gas-sensitive materials, but the hydrogen sensing performance of the material cannot meet the requirement of hydrogen detection. To build up SnO2And other metal oxide heterostructures, it is possible to improve the sensing performance through the fermi level control effect and the synergistic effect among different components. By utilizing the surface characteristics and small size effect of the nano particles, the selectivity, stability and sensitivity of the sensing material can be effectively improved, and the response-recovery time is reduced.
The coprecipitation method is one of the common methods for preparing small-size nano powder materials, and has the characteristics of simple operation, mild conditions, short synthesis period and suitability for batch production. At present, the method is still mainly used for synthesizing small-size nano powder materials in industry. Therefore, the coprecipitation method is adopted to prepare the nano-scale SnO2The hydrogen sensing material with the base heterostructure has important practical application value and practical significance.
In bookIn the invention, we prepared a CdO/SnO2A composite nanocube gas sensitive material. The material is simple in preparation process, easy for large-scale production, excellent in sensing sensitivity, selectivity, quick response and the like, and can be used for quick detection of low-concentration hydrogen.
Disclosure of Invention
The invention aims to provide a CdO/SnO2A composite nanocube gas-sensitive material, a preparation method and application thereof in hydrogen detection. The invention takes stannic chloride hydrate and cadmium dichloride hydrate as metal raw materials and takes sodium hydroxide and sodium carbonate mixed solution as a precipitator to prepare a series of CdO/SnO with different molar ratios2And compounding the gas-sensitive material of nanocubes (80-100 nm). The series of materials have the advantages of low detection limit, high sensitivity, good selectivity, short response-recovery time and the like in the aspect of detecting hydrogen, can be used for monitoring and early warning of hydrogen leakage, and have the advantages of simple synthesis condition, short preparation period, low raw material cost, easiness in realizing large-scale production and the like.
The invention relates to CdO/SnO2The preparation method of the composite nanocube gas-sensitive material comprises the following steps:
(1) preparation of a precipitant solution: the molar ratio is (0.25-1): 1 sodium carbonate (Na)2CO3) And sodium hydroxide (NaOH) are added into deionized water to be dissolved;
(2) preparing a metal salt mixed solution: mixing a mixture of 1: (0.25-4) tin tetrachloride (SnCl)4·5H2O) and cadmium chloride (CdCl)2·2.5H2O) adding the mixture into deionized water for dissolving, and stirring the mixture at room temperature until the mixture is uniform;
(3) dropwise and slowly adding the precipitator prepared in the step (1) into the solution prepared in the step (2), stopping dropwise adding when the pH value is 6-12, and continuously stirring;
(4) after the precipitation in the step (3) is completed, carrying out centrifugal separation and water washing on the reaction product for 3-5 times, and drying to obtain a precursor;
(5) sintering the precursor obtained in the step (4) in a muffle furnace to obtain the CdO/SnO2CompoundingA nanocube gas sensitive material.
In the method, in the deionized water in the step (1), the concentration of sodium hydroxide (NaOH) is 0.5-2 mol/L;
in the method, in the deionized water in the step (2), tin tetrachloride (SnCl)4·5H2O) with a concentration of 0.005-0.05 mol/L;
in the method, the continuous stirring time in the step (3) is 1-10 hours.
In the method, the drying temperature in the step (4) is 60-80 ℃, and the drying time is 5-12 hours.
In the method, the sintering temperature in the step (5) is 300-500 ℃, the heating rate is 2-5 ℃/min, and the sintering time is 1-3 hours.
The gas sensor is formed by Al with two parallel annular gold electrodes separated from each other on the outer surface2O3Ceramic tube coated with Al2O3CdO/SnO on ceramic tube external surface and gold electrode2Composite nanocube gas-sensitive material (the thickness of the gas-sensitive material is 20 μm) placed in Al2O3A nickel-chromium heating coil (with a resistance value of 30 omega) in the ceramic tube; two platinum wires are led out from each gold electrode, two platinum wires are led out from two ends of the nickel-chromium heating coil, the nickel-chromium alloy heating wire is used as a heating body to control the working temperature of the sensor, and Al2O3The ceramic tube is welded on the hexagonal base through six platinum wires.
The invention has the following advantages:
1. the invention relates to CdO/SnO2The composite nanocube gas-sensitive material has the advantages of simple preparation method, easy realization of synthesis conditions, short synthesis period, low raw material cost and easy realization of large-scale production.
2. The invention relates to CdO/SnO2The composite nanocube gas-sensitive material utilizes the characteristics of nanoparticles, and improves the sensing performance of hydrogen detection from the aspect of size effect.
3. The invention relates to CdO/SnO2The composite nanocube gas-sensitive material realizes the adjustment of an electronic structure by constructing a heterostructure so as to improve the detection of hydrogenSensing performance.
4. The invention relates to CdO/SnO2The composite nanocube gas-sensitive material has the advantages of high detection sensitivity, high response-recovery speed and the like in the aspect of detecting hydrogen. This greatly helps the quick detection and the early warning in time to hydrogen, provides the assurance for the safe handling of hydrogen.
Drawings
FIG. 1: a series of CdO/SnO with different molar ratios2Composite nanocube gas-sensitive material, and CdO and SnO2Powder X-ray diffraction (XRD) pattern of pure phase and its standard XRD card.
FIG. 2: CdO/SnO obtained in example 12(molar ratio 1:1) Scanning Electron Microscope (SEM) picture of the composite nanocube gas-sensitive material, wherein the particle size is 80-100 nm.
FIG. 3: CdO/SnO obtained in example 22(molar ratio 2:1) Scanning Electron Microscope (SEM) picture of the composite nanocube gas-sensitive material, wherein the particle size is 80-100 nm.
FIG. 4: CdO/SnO obtained in example 32(molar ratio 1:2) Scanning Electron Microscope (SEM) picture of the composite nanocube gas-sensitive material, wherein the particle size is 80-100 nm.
Fig. 5 (a): CdO/SnO obtained in example 12Response-recovery curve of composite nanocube gas sensitive material to 500ppm hydrogen. At the working temperature of 220 ℃, the response value is 19, and both the response time and the recovery time are less than 5 s.
Fig. 5 (B): CdO/SnO obtained in example 12Response-recovery curve of composite nanocube gas sensitive material to 10ppm hydrogen. At an operating temperature of 220 ℃, the response value is 2.6, which indicates that the detection lower limit is low, and hydrogen leakage can be effectively monitored. The response value is the ratio (S ═ Ra/Rg) of the resistance (Ra) between the two gold electrodes of the gas sensor in the air atmosphere and the resistance (Rg) between the two gold electrodes of the gas sensor in the atmosphere to be measured.
FIG. 6: CdO/SnO obtained in example 12And (3) a histogram of response values of the composite nanocube gas-sensitive material to 500ppm of different gases. At 220 deg.C, the material can be used for treating CO, methane, ethane, propane, ethylene, etcThe body is essentially non-responsive, indicating that it has an excellent specific response to hydrogen.
Detailed Description
The present invention is further illustrated by the following examples, but the scope of the present invention is not limited to the following examples. It will be apparent to those skilled in the art that variations or modifications of the present invention can be made without departing from the spirit and scope of the invention, and these variations or modifications are also within the scope of the invention.
Example 1: CdO/SnO with molar ratio of 1:12And (3) preparing the composite nanocube gas-sensitive material.
(1) 4g of sodium hydroxide (NaOH) and 5.3g of sodium carbonate (Na) are weighed out2CO3) The molar ratio is 2:1, the sodium hydroxide (NaOH) is dissolved in 100mL deionized water to prepare sodium carbonate (Na) with the concentration of 1mol/L2CO3) Mixed solution with the concentration of 0.5mol/L is used as a precipitator;
(2) 0.1461g of tin tetrachloride pentahydrate (SnCl) were weighed out4·5H2O) and 0.0951g of cadmium chloride pentahydrate (CdCl) in two points2·2.5H2O), the molar ratio is 1:1, dissolving in 50mL of deionized water to prepare tin tetrachloride pentahydrate (SnCl)4·5H2O) concentration of 0.0167mol/L, cadmium chloride pentahydrate two-point (CdCl)2·2.5H2O) mixed solution with the concentration of 0.0167mol/L is stirred to be uniform at room temperature;
(3) dropwise and slowly adding the precipitator prepared in the step (1) into the solution prepared in the step (2), stopping dropwise adding when the pH value is 11, and continuously stirring for 5 hours;
(4) after the precipitation is completed, carrying out centrifugal separation and washing on the reaction product for three times, and then placing the reaction product in a drying oven at 80 ℃ for drying for 12 hours;
(5) putting the precursor obtained after drying in the step (4) into a muffle furnace, heating to 400 ℃ at the speed of 3 ℃/min, and sintering for 2 hours to finally obtain the gas-sensitive material for rapidly detecting hydrogen, wherein the gas-sensitive material is CdO/SnO with the molar ratio of 1:12A composite nanocube.
Example 2: CdO/SnO with molar ratio of 2:12And (3) preparing the composite nanocube gas-sensitive material.
(1) 4g of sodium hydroxide (NaOH) and 5.3g of sodium carbonate (Na) are weighed out2CO3) The molar ratio is 2:1, the sodium hydroxide (NaOH) is dissolved in 100mL deionized water to prepare sodium carbonate (Na) with the concentration of 1mol/L2CO3) Mixed solution with the concentration of 0.5mol/L is used as a precipitator;
(2) 0.1268g of cadmium chloride pentahydrate (CdCl) were weighed out2·2.5H2O) and 0.0974g of tin tetrachloride pentahydrate (SnCl)4·5H2O) with the molar ratio of 2:1, dissolving in 50mL of deionized water to prepare tin tetrachloride pentahydrate (SnCl)4·5H2O) concentration of 0.0056mol/L, two-point pentahydrate cadmium chloride (CdCl)2·2.5H2O) mixed solution with the concentration of 0.0111mol/L is stirred to be uniform at room temperature;
(3) dropwise and slowly adding the precipitator prepared in the step (1) into the solution prepared in the step (2), stopping dropwise adding when the pH value is 11, and continuously stirring for 5 hours;
(4) after the precipitation is completed, carrying out centrifugal separation and washing on the reaction product for three times, and then placing the reaction product in a drying oven at 80 ℃ for drying for 12 hours;
(5) putting the precursor obtained after drying in the step (4) into a muffle furnace, heating to 400 ℃ at the speed of 3 ℃/min, and sintering for 2 hours to finally obtain the gas-sensitive material for rapidly detecting hydrogen, wherein the gas-sensitive material is CdO/SnO with the molar ratio of 2:12A composite nanocube.
Example 3: CdO/SnO with molar ratio of 1:22And (3) preparing the composite nanocube gas-sensitive material.
(1) 4g of sodium hydroxide (NaOH) and 5.3g of sodium carbonate (Na) are weighed out2CO3) The molar ratio is 2:1, the sodium hydroxide (NaOH) is dissolved in 100mL deionized water to prepare sodium carbonate (Na) with the concentration of 1mol/L2CO3) Mixed solution with the concentration of 0.5mol/L is used as a precipitator;
(2) 0.0634g of cadmium chloride pentahydrate (CdCl) was weighed out2·2.5H2O) and 0.1948g of tin tetrachloride pentahydrate (SnCl)4·5H2O), MoDissolving the raw materials in 50mL of deionized water at a molar ratio of 1:2 to prepare tin tetrachloride pentahydrate (SnCl)4·5H2O) concentration of 0.0111mol/L, cadmium chloride (CdCl) pentahydrate at two points2·2.5H2O) mixed solution with the concentration of 0.0056mol/L is stirred to be uniform at room temperature;
(3) dropwise and slowly adding the precipitator prepared in the step (1) into the solution prepared in the step (2), stopping dropwise adding when the pH value is 11, and continuously stirring for 5 hours;
(4) after the precipitation is completed, carrying out centrifugal separation and washing on the reaction product for three times, and then placing the reaction product in a drying oven at 80 ℃ for drying for 12 hours;
(5) putting the precursor obtained after drying in the step (4) into a muffle furnace, heating to 400 ℃ at the speed of 3 ℃/min, and sintering for 2 hours to finally obtain the gas-sensitive material for rapidly detecting hydrogen, wherein the gas-sensitive material is CdO/SnO with the molar ratio of 1:22A composite nanocube.
Claims (8)
1. CdO/SnO2The preparation method of the composite nanocube gas-sensitive material comprises the following steps:
(1) preparation of a precipitant solution: the molar ratio is (0.25-1): 1, adding sodium carbonate and sodium hydroxide into deionized water for dissolving;
(2) preparing a metal salt mixed solution: mixing a mixture of 1: (0.25-4) adding tin tetrachloride and cadmium chloride into deionized water for dissolving, and stirring at room temperature until the mixture is uniform;
(3) dropwise and slowly adding the precipitator prepared in the step (1) into the solution prepared in the step (2), stopping dropwise adding when the pH value is 6-12, and continuously stirring;
(4) after the precipitation in the step (3) is completed, carrying out centrifugal separation and water washing on the reaction product for 3-5 times, and drying to obtain a precursor;
(5) sintering the precursor obtained in the step (4) to obtain the CdO/SnO2A composite nanocube gas sensitive material.
2. The CdO/SnO according to claim 12Composite nanocubeThe preparation method of the gas sensitive material is characterized by comprising the following steps: in the deionized water in the step (1), the concentration of the sodium hydroxide is 0.5-2 mol/L.
3. The CdO/SnO according to claim 12The preparation method of the composite nanocube gas-sensitive material is characterized by comprising the following steps: in the deionized water in the step (2), the concentration of the stannic chloride is 0.005-0.05 mol/L.
4. The CdO/SnO according to claim 12The preparation method of the composite nanocube gas-sensitive material is characterized by comprising the following steps: and (4) continuously stirring for 1-10 hours in the step (3).
5. The CdO/SnO according to claim 12The preparation method of the composite nanocube gas-sensitive material is characterized by comprising the following steps: the drying temperature of the step (4) is 60-80 ℃, and the drying time is 5-12 hours.
6. The CdO/SnO according to claim 12The preparation method of the composite nanocube gas-sensitive material is characterized by comprising the following steps: the sintering temperature in the step (5) is 300-500 ℃, the heating rate is 2-5 ℃/min, and the sintering time is 1-3 hours.
7. CdO/SnO2The composite nanocube gas-sensitive material is characterized in that: is prepared by the method of any one of claims 1 to 6.
8. A CdO/SnO according to claim 72The application of the composite nanocube gas-sensitive material in hydrogen detection.
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| CN115477323A (en) * | 2022-10-08 | 2022-12-16 | 吉林大学 | Mesoporous indium tin oxide microsphere gas-sensitive material, preparation method and application thereof in hydrogen detection |
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| CN109019673A (en) * | 2018-08-01 | 2018-12-18 | 济南大学 | A kind of SnO2-In2O3The preparation method of nanocomposite |
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| CN109019673A (en) * | 2018-08-01 | 2018-12-18 | 济南大学 | A kind of SnO2-In2O3The preparation method of nanocomposite |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115477323A (en) * | 2022-10-08 | 2022-12-16 | 吉林大学 | Mesoporous indium tin oxide microsphere gas-sensitive material, preparation method and application thereof in hydrogen detection |
| CN115477323B (en) * | 2022-10-08 | 2023-06-27 | 吉林大学 | Mesoporous indium tin oxide microsphere gas-sensitive material, preparation method and application thereof in hydrogen detection |
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