CN112816525B - Preparation method of semiconductor gas sensor for seafood freshness detection - Google Patents
Preparation method of semiconductor gas sensor for seafood freshness detection Download PDFInfo
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- CN112816525B CN112816525B CN202011625478.5A CN202011625478A CN112816525B CN 112816525 B CN112816525 B CN 112816525B CN 202011625478 A CN202011625478 A CN 202011625478A CN 112816525 B CN112816525 B CN 112816525B
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- 239000004065 semiconductor Substances 0.000 title claims abstract description 19
- 235000014102 seafood Nutrition 0.000 title claims abstract description 16
- 238000001514 detection method Methods 0.000 title claims abstract description 8
- 238000002360 preparation method Methods 0.000 title claims abstract description 5
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000011258 core-shell material Substances 0.000 claims abstract description 21
- 239000002086 nanomaterial Substances 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000002002 slurry Substances 0.000 claims abstract description 8
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims abstract description 7
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229940116411 terpineol Drugs 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000005516 engineering process Methods 0.000 claims abstract description 4
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 4
- 239000010703 silicon Substances 0.000 claims abstract description 4
- 239000000758 substrate Substances 0.000 claims abstract description 4
- 239000007864 aqueous solution Substances 0.000 claims description 30
- 239000011259 mixed solution Substances 0.000 claims description 18
- YZYKBQUWMPUVEN-UHFFFAOYSA-N zafuleptine Chemical compound OC(=O)CCCCCC(C(C)C)NCC1=CC=C(F)C=C1 YZYKBQUWMPUVEN-UHFFFAOYSA-N 0.000 claims description 15
- YSWBFLWKAIRHEI-UHFFFAOYSA-N 4,5-dimethyl-1h-imidazole Chemical compound CC=1N=CNC=1C YSWBFLWKAIRHEI-UHFFFAOYSA-N 0.000 claims description 14
- 239000000047 product Substances 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000002244 precipitate Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 229910020599 Co 3 O 4 Inorganic materials 0.000 claims description 5
- QCAZZPKUBLATEK-UHFFFAOYSA-L cobalt(2+) diacetate dihydrate Chemical compound O.O.[Co+2].CC([O-])=O.CC([O-])=O QCAZZPKUBLATEK-UHFFFAOYSA-L 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 15
- 238000011084 recovery Methods 0.000 abstract description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 10
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 abstract 1
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 59
- 230000035945 sensitivity Effects 0.000 description 18
- 229910021529 ammonia Inorganic materials 0.000 description 4
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 3
- 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 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (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)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The invention discloses a kind ofThe invention discloses a preparation method of a semiconductor gas sensor for seafood freshness detection, and develops a semiconductor core-shell structure nanomaterial Co with ultra-fast response and good selectivity to trimethylamine gas 3 O 4 The @ ZnO material is prepared by oxidizing a core-shell structure ZIF67@ZIF8 and has a porous and hollow structure; uniformly mixing and grinding the Co3O4@ZnO nano material and terpineol to form slurry with certain viscosity; and (3) adopting a silicon substrate interdigital electrode chip integrated with a micro-heater based on MEMS technology as a sensor chip, and coating the prepared slurry on the middle position of the interdigital electrode to obtain the sensor device with stable performance. The sensor prepared by the invention has good selectivity when detecting trimethylamine gas, is not interfered by ethanol, ammonia gas and the like, is little influenced by environmental humidity, and has rapid response and thorough recovery.
Description
Technical Field
The invention relates to a semiconductor gas sensor, in particular to a semiconductor gas sensor for detecting the freshness of seafood.
Background
The seafood products are extremely easy to spoil, trimethylamine gas can be generated when the seafood products are lengthened along with the placement time, and the freshness of the seafood products can be detected through the concentration of the trimethylamine gas. The conventional trimethylamine semiconductor gas sensor has poor selectivity, higher detection concentration and longer response/recovery time, and limits the application of the trimethylamine semiconductor gas sensor.
Disclosure of Invention
Aiming at the defects of the prior art, the invention develops a semiconductor gas-sensitive material with ultra-high sensitivity and selectivity to trimethylamine gas through the design of a core-shell structure nano material, and prepares the semiconductor gas sensor for detecting the freshness of seafood.
The preparation method of the semiconductor gas sensor for detecting the freshness of the seafood specifically comprises the following steps:
preparing a certain concentration of cobalt acetate dihydrate aqueous solution and dimethyl imidazole aqueous solution respectively, taking a certain amount of zinc acetate dihydrate aqueous solution and dimethyl imidazole aqueous solution respectively, fully and uniformly mixing the two aqueous solutions in equal volume, standing the obtained mixed solution at room temperature for 30min, centrifugally separating precipitate in the mixed solution, washing, and drying under vacuum condition to obtain a product ZIF67;
step two, taking a certain amount of the product in the step 1, and dispersing the product into a dimethyl imidazole water solution to obtain a mixed solution A;
and thirdly, preparing a zinc acetate dihydrate water solution with a certain concentration, adding the zinc acetate dihydrate water solution into the mixed solution A obtained in the step 2, mixing the zinc acetate dihydrate water solution and the mixed solution A in equal volume, and then placing the mixture at room temperature for 30min after fully and uniformly mixing the zinc acetate dihydrate water solution and the mixed solution A. And centrifugally separating, washing and vacuum drying the precipitate in the mixed solution to obtain the ZIF67@ZIF8 with the core-shell nano structure.
Calcining the ZIF core-shell structure nano material prepared in the step 3 in air to obtain porous hollow Co 3 O 4 @zno core-shell structure.
Step five, co prepared in the step 4 is mixed 3 O 4 Grinding and mixing the nano material with the @ ZnO core-shell structure and terpineol uniformly to form slurry with certain viscosity; the MEMS technology-based silicon substrate interdigital electrode chip integrated with the micro-heater is adopted as a sensor chip, the prepared slurry is coated at the middle position of the interdigital electrode, and the integrated micro-heater is utilized to remove the organic solvent terpineol, so that the sensitive material Co is prepared 3 O 4 The semiconductor gas sensor of@ZnO has ultrasensitive selectivity specificity to trimethylamine gas and can be used for detecting the freshness of seafood.
Preferably, the synthesis of the ZIF67@ZIF8 core-shell structure takes ZIF67 as a core and ZIF8 as an outer shell, wherein the ZIF67 is synthesized in the step 1, and the ZIF8 shell is wrapped on the surface of the ZIF67 in the step three.
Preferably, the concentration of the cobalt acetate dihydrate aqueous solution in the first step and the third step is 120mmol/L; the concentration of the dimethylimidazole aqueous solution is 6mol/L.
Preferably, the amounts of the zinc acetate dihydrate aqueous solution and the dimethyl imidazole aqueous solution are respectively 8-10mL.
The beneficial effects are that:
1. the gas sensor prepared by the invention has good selective detectability on trimethylamine gas;
2. the gas sensor prepared by the invention has ultra-rapid detection characteristic on low-concentration trimethylamine gas, and has higher sensitivity;
3. when the gas sensor prepared by the invention detects low-concentration trimethylamine gas, the gas sensor is hardly influenced by high-concentration formaldehyde, ethanol, ammonia gas and other gases.
4. When the gas sensor prepared by the invention detects trimethylamine gas, the gas sensor is little influenced by environmental humidity.
Drawings
FIG. 1 is Co prepared in example 1 3 O 4 Nano material with @ ZnO core-shell structure;
FIG. 2 is a comparison of sensitivity of the gas sensor prepared in example 1 to trimethylamine, formaldehyde, ethanol and ammonia gases;
FIG. 3 is a plot of the sensitivity response/recovery of the gas sensor prepared in example 1 to trimethylamine gases of different concentrations;
FIG. 4 is a plot of the sensitivity response/recovery of the gas sensor prepared in example 1 to trimethylamine gas at various humidities;
FIG. 5 is a plot of the sensitivity response/recovery of the gas sensor prepared in example 1 against 33ppm trimethylamine gas;
FIG. 6 is a plot of the sensitivity response/recovery of the gas sensor prepared in example 2 to trimethylamine gases of different concentrations.
Detailed Description
Example 1
1) Preparing cobalt acetate dihydrate aqueous solution with the concentration of 120mmol/L and dimethyl imidazole aqueous solution with the concentration of 6mol/L respectively, taking 10mL of zinc acetate dihydrate aqueous solution and dimethyl imidazole aqueous solution respectively, fully and uniformly mixing the two aqueous solutions in equal volumes, standing the obtained mixed solution for 30min at room temperature, centrifugally separating precipitate in the mixed solution, washing, and drying under vacuum conditions to obtain a product ZIF67;
2) Dispersing 20mg of the product obtained in the step 1 into 5mL of 1.9mol/L dimethyl imidazole water solution to obtain a mixed solution A;
3) And (2) adding 120mmol/L zinc acetate dihydrate aqueous solution into the mixed solution A obtained in the step (2), wherein the volume ratio of the zinc acetate dihydrate aqueous solution to the solution A is 1:1, and standing for 30min at room temperature after fully and uniformly mixing. And centrifugally separating, washing and vacuum drying the precipitate in the mixed solution to obtain the ZIF67@ZIF8 with the core-shell nano structure.
4) Calcining the ZIF core-shell structure nano material prepared in the step 3 in air at 400 ℃ for 2 hours, wherein the heating rate is 1 ℃/min, and obtaining porous and hollow Co 3 O 4 @zno core-shell structure.
5) Co prepared in step 4 3 O 4 The weight ratio of the nano material with the @ ZnO core-shell structure to terpineol is 5:1, grinding and mixing uniformly to form slurry with certain viscosity; the MEMS technology-based silicon substrate interdigital electrode chip integrated with the micro-heater is adopted as a sensor chip, the prepared slurry is coated at the middle position of the interdigital electrode, and the integrated micro-heater is utilized to remove the organic solvent terpineol, so that the sensitive material Co is prepared 3 O 4 The semiconductor gas sensor of@ZnO has ultrasensitive selectivity specificity to trimethylamine gas and can be used for detecting the freshness of seafood.
Co prepared in example 1 3 O 4 The @ ZnO core-shell structure is shown in figure 1, and the inner core is Co 3 O 4 The shell is ZnO;
the sensitivity of the gas sensor prepared in example 1 to trimethylamine, formaldehyde, ethanol and ammonia is compared with that of the gas sensor shown in fig. 2, and the gas sensor has good selectivity to low-concentration trimethylamine gas;
the sensitivity response/recovery curves of the gas sensor prepared in example 1 to trimethylamine gases with different concentrations are shown in fig. 3, and when the gas sensor contacts with trimethylamine gases, the current of the sensor rises rapidly and reaches stability quickly, and the response time for detecting the trimethylamine gases with different concentrations is about 3 s; after the trimethylamine gas is removed, the current of the sensor is rapidly reduced to an initial value, and the recovery time after the trimethylamine gas with different concentrations is detected is about 2 s; the sensitivity to 33ppm trimethylamine gas was about 42, and when the concentration exceeded 33ppm, the value of the sensitivity tended to saturate.
The sensitivity response/recovery curves of the gas sensor prepared in example 1 to 33ppm trimethylamine gas at 60%, 70%, 80% different humidity are shown in fig. 4, and the influence of ambient humidity on the sensor sensitivity at the operating temperature of 250 ℃ is small, and the sensitivity fluctuation value is about 6%.
The repeatability sensitive response/recovery curve of the gas sensor prepared in example 1 to 33ppm trimethylamine gas is shown in fig. 5, the repeatability of the sensor for detecting trimethylamine gas is good, the cross sensitivity to ethanol and ammonia is weak, and the sensor is hardly influenced by ethanol and ammonia when detecting trimethylamine.
Example 2
This example is similar to example 1 except that 5mg of the product of step 1) is taken in step 2) and dispersed into 5mL of an aqueous solution of dimethylimidazole having a concentration of 1.9mol/L to give a mixed solution A.
The sensitivity response/recovery curves of the gas sensor prepared in example 2 for trimethylamine gases of different concentrations are shown in fig. 6.
Example 3
The example is similar to example 1, except that step 4) the ZIF core-shell structure nanomaterial prepared in step 3 is calcined in air at 380 ℃ for 2 hours at a heating rate of 1.5 ℃/min to obtain porous and hollow Co 3 O 4 @zno core-shell structure.
The invention adopts a static gas distribution method to measure the sensitivity characteristic of a semiconductor sensor, and the sensitivity when detecting gas is defined as (I) s -I 0 )/I 0 Wherein I s Indicating the current value of the sensor in a gas to be detected with a certain concentration ， I 0 Indicating the current value of the sensor in the background gas.
Claims (4)
1. The preparation method of the semiconductor gas sensor for detecting the freshness of the seafood is characterized by comprising the following steps of:
preparing a cobalt acetate dihydrate aqueous solution and a dimethyl imidazole aqueous solution respectively, taking a zinc acetate dihydrate aqueous solution and a dimethyl imidazole aqueous solution, fully and uniformly mixing the two aqueous solutions in equal volume, standing the obtained mixed solution at room temperature for 30min, centrifugally separating a precipitate in the mixed solution, washing, and drying under vacuum conditions to obtain a product ZIF67;
step two, taking 5-20mg of the product in the step 1, and dispersing the product into 4-6mL of dimethyl imidazole water solution with the concentration of 1.9mol/L to obtain a mixed solution A;
step three, taking a certain amount of zinc acetate dihydrate aqueous solution with the concentration of 120mmol/L, adding the zinc acetate dihydrate aqueous solution into the mixed solution A obtained in the step 2, wherein the volume ratio of the zinc acetate dihydrate aqueous solution to the solution A is 1:1, and fully and uniformly mixing the zinc acetate dihydrate aqueous solution and the solution A, and then standing the mixture at room temperature for 30min; centrifugally separating, washing and vacuum drying the precipitate in the mixed solution to obtain ZIF67@ZIF8 with a core-shell nano structure;
calcining the ZIF core-shell structure nano material prepared in the step 3 in air at 350-450 ℃ for 2h, wherein the heating rate is 1-2 ℃/min, and obtaining the porous hollow Co 3 O 4 A @ ZnO core-shell structure;
step five, co prepared in the step 4 is mixed 3 O 4 Grinding and mixing the nano material with the @ ZnO core-shell structure and terpineol uniformly to form slurry with viscosity; the MEMS technology-based silicon substrate interdigital electrode chip integrated with the micro-heater is adopted as a sensor chip, the prepared slurry is coated at the middle position of the interdigital electrode, and the integrated micro-heater is utilized to remove the organic solvent terpineol, so that the sensitive material Co is prepared 3 O 4 The semiconductor gas sensor of@ZnO has ultrasensitive selectivity specificity to trimethylamine gas and can be used for detecting the freshness of seafood.
2. The method for preparing the semiconductor gas sensor for seafood freshness detection according to claim 1, wherein the synthesis of the ZIF67@ZIF8 core-shell structure is characterized in that ZIF67 is taken as a core and ZIF8 is taken as an outer shell, the ZIF67 is synthesized in the step 1, and a ZIF8 shell is wrapped on the surface of the ZIF67 in the step three.
3. The method for preparing a semiconductor gas sensor for seafood freshness detection according to claim 1, wherein the concentration of cobalt acetate dihydrate aqueous solution in the first and third steps is 120mmol/L; the concentration of the dimethylimidazole aqueous solution is 6mol/L.
4. The method for preparing a semiconductor gas sensor for seafood freshness detection according to claim 3, wherein the amounts of the zinc acetate dihydrate aqueous solution and the dimethyl imidazole aqueous solution are respectively 8-10mL.
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| CN113433172B (en) * | 2021-06-25 | 2022-11-04 | 杭州电子科技大学 | Preparation method of novel ammonia gas sensor based on MOFs (metal-organic frameworks) material |
| CN113562775B (en) * | 2021-08-30 | 2023-06-30 | 杭州恒毅智创科技有限公司 | Preparation method of zinc oxide/cobaltosic oxide hollow cube nanomaterial |
| CN117737887B (en) * | 2024-02-16 | 2024-05-10 | 天津市计量监督检测科学研究院 | Preparation method and application of composite nanofiber gas-sensitive material |
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| CN111307880A (en) * | 2020-02-18 | 2020-06-19 | 杭州电子科技大学 | Preparation method of organic volatile gas sensor based on MOF core-shell nanostructure |
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| Synthesis of Co3O4/ZnO nano-heterojunctions by one-off processing ZIF-8@ZIF-67 and their gas-sensing performances for trimethylamine;Yuanyuan Li;Sensors and Actuators B: Chemical;第1-9页 * |
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