CN113447533B - Ni-SnO with urea as additive for low-power consumption formaldehyde detection 2 Preparation method of gas-sensitive material - Google Patents
Ni-SnO with urea as additive for low-power consumption formaldehyde detection 2 Preparation method of gas-sensitive material Download PDFInfo
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- CN113447533B CN113447533B CN202110727943.4A CN202110727943A CN113447533B CN 113447533 B CN113447533 B CN 113447533B CN 202110727943 A CN202110727943 A CN 202110727943A CN 113447533 B CN113447533 B CN 113447533B
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- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 title claims abstract description 84
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 239000004202 carbamide Substances 0.000 title claims abstract description 19
- 239000000463 material Substances 0.000 title claims abstract description 15
- 239000000654 additive Substances 0.000 title claims abstract description 13
- 230000000996 additive effect Effects 0.000 title claims abstract description 13
- 238000001514 detection method Methods 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 230000004044 response Effects 0.000 claims abstract description 13
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 7
- 239000000758 substrate Substances 0.000 claims abstract description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000011084 recovery Methods 0.000 claims abstract description 6
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 4
- 239000011248 coating agent Substances 0.000 claims abstract description 4
- 238000000576 coating method Methods 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 230000032683 aging Effects 0.000 claims description 11
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 9
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- 239000011258 core-shell material Substances 0.000 claims description 2
- 230000035945 sensitivity Effects 0.000 abstract description 8
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 230000002431 foraging effect Effects 0.000 abstract description 3
- 238000005303 weighing Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 28
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 9
- 238000000034 method Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000011540 sensing material Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 102000003839 Human Proteins Human genes 0.000 description 1
- 108090000144 Human Proteins Proteins 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- -1 hydroxide ions Chemical class 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000000622 irritating effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 210000004400 mucous membrane Anatomy 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000004867 photoacoustic spectroscopy Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- CVNKFOIOZXAFBO-UHFFFAOYSA-J tin(4+);tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[Sn+4] CVNKFOIOZXAFBO-UHFFFAOYSA-J 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
The invention discloses Ni-SnO with urea as an additive for low-power consumption formaldehyde detection 2 A preparation method of a gas-sensitive material belongs to the technical field of formaldehyde detection and comprises the following steps: weighing SnCl 4 ·5H 2 O、NiCl 2 ·6H 2 Stirring O and urea into deionized water to dissolve completely; pouring the solution into a hydrothermal kettle, and reacting at constant temperature; cooling to room temperature, filtering and washing; placing the mixture into an oven for aging; alumina ceramic silver-plated electrodes with electrode spacing of 0.15mm, electrode width of 0.18mm and film thickness of 5-11 μm; respectively ultrasonically treating the substrate electrode in ethanol and deionized water for 3min, and drying; mixing the aged powder with ethanol reagent, and coating on a substrate electrode; placing the mixture into an oven for aging. The invention can obtain uniform Ni-SnO with large specific surface area by using urea additive with lower cost 2 The formaldehyde gas-sensitive device prepared from the gas-sensitive material has the advantages of low working temperature, low energy consumption, short response and recovery time, high sensitivity, good selectivity and good stability.
Description
Technical Field
The invention belongs to the technical field of formaldehyde detection, and in particular relates to Ni-SnO with urea used for low-power consumption formaldehyde detection as an additive 2 A preparation method of a gas-sensitive material.
Background
With the development of industry in recent years, the detection problem of various gases, especially various harmful gases affecting our daily lives, needs to be particularly emphasized. Formaldehyde is listed by the international cancer research institute as a serious carcinogen. Formaldehyde has a strong irritating effect on skin and mucous membranes of the body (such as nose, sound and eye mask) and can even denature human protein coagulation.
At present, the monitoring of target gas mainly comprises a gas chromatography method, an infrared spectrometry method, a photoacoustic spectrometry method and a gas-sensitive sensing element method, and the methods have the problems of complex operation, high price, long period, high power consumption, high working temperature and the like.
Tin dioxide is a wide band gap semiconductor with a potential difference of 3-6eV at 300K. As an important semiconductor sensing material, the sensor has high sensitivity to various combustible gases, industrial waste gases, polluted gases and other gases, and is often used for manufacturing gas sensors.
However, pure tin dioxide materials have undesirable sensitivity and selectivity to formaldehyde. While the noble metal modified tin dioxide can improve the gas sensitivity of the tin oxide gas sensitive material, the noble metal modified tin dioxide causes the problems of rapid increase of cost, environmental pollution and the like. In summary, the existing semiconductor gas sensor has the defects of high working temperature, high energy consumption and the like, and the gas sensing material with high formaldehyde sensitivity, good selectivity and low cost at a lower working temperature is continuously further developed.
Disclosure of Invention
The invention aims at solving the existing problems and provides Ni-SnO with urea used for low-power consumption formaldehyde detection as an additive 2 A preparation method of a gas-sensitive material.
The invention is realized by the following technical scheme:
Ni-SnO with urea as additive for low-power consumption formaldehyde detection 2 The preparation method of the gas-sensitive material comprises the following steps:
the first step: weigh 8.75g SnCl 4 ·5H 2 O、0.59gNiCl 2 ·6H 2 Dissolving O and 2.65g of urea into 20ml of deionized water, stirring to completely dissolve, and performing ultrasonic treatment for 15min;
and a second step of: pouring the solution into a hydrothermal kettle, and reacting for 12 hours at the constant temperature of 180 ℃;
and a third step of: after cooling to room temperature, filtering and washing 3 times;
fourth step: aging in an oven to obtain white SnO 2 (NH 3 ·H 2 O) powder;
fifth step: alumina ceramic silver-plated electrodes with electrode spacing of 0.15mm, electrode width of 0.18mm and film thickness of 5-11 μm;
sixth step: respectively ultrasonically treating the substrate electrode in ethanol and deionized water for 3min, and drying in a drying oven;
seventh step: mixing the aged powder with ethanol reagent, and coating on a substrate electrode;
eighth step: and (5) putting the mixture into an oven for aging.
Further, the aging treatment in the fourth step is aging at a constant temperature of 60 ℃ for 24 hours.
Further, the drying in the sixth step is carried out at a constant temperature of 50 ℃.
Further, the aging in the eight steps is aging for 24 hours at a constant temperature of 40 ℃.
Compared with the prior art, the invention has the following advantages:
with the scheme, the urea with low power consumption formaldehyde detection is used as Ni-SnO of the additive 2 The gas-sensitive material and the preparation method thereof have the following advantages:
1. the invention can obtain uniform Ni-SnO with large specific surface area by using urea additive with lower cost 2 The formaldehyde gas-sensitive device prepared from the gas-sensitive material has the advantages of low working temperature, low energy consumption, short response and recovery time, high sensitivity, good selectivity and good stability;
2. the method has the advantages of simple preparation process, wide raw material sources, low cost, high yield and easy realization of industrial production and application, and the process is operated and controlled.
Drawings
FIG. 1 shows Ni-SnO prepared by a hydrothermal method using urea as an additive in the present application 2 SEM image of the sample;
FIG. 2 shows the Ni-SnO at different operating temperatures in the present application 2 Response to formaldehyde;
FIG. 3 is a diagram of Ni-SnO in the present application 2 Response characteristics at different concentrations of formaldehyde;
FIG. 4 is a diagram of Ni-SnO in the present application 2 Response to formaldehyde and recovery time;
FIG. 5 is a diagram of Ni-SnO in the present application 2 Selectivity to formaldehyde gas.
Detailed Description
Ni-SnO with urea as additive for low-power consumption formaldehyde detection 2 The preparation method of the gas-sensitive material comprises the following steps:
the first step: weigh 8.75g SnCl 4 ·5H 2 O、0.59gNiCl 2 ·6H 2 Dissolving O and 2.65g of urea into 20ml of deionized water, stirring to completely dissolve, and performing ultrasonic treatment for 15min;
and a second step of: pouring the solution into a hydrothermal kettle, and reacting for 12 hours at the constant temperature of 180 ℃;
and a third step of: after cooling to room temperature, filtering and washing 3 times;
fourth step: aging in oven at 60deg.C for 24 hr to obtain white SnO 2 (NH 3 ·H 2 O) powder;
fifth step: alumina ceramic silver-plated electrodes with electrode spacing of 0.15mm, electrode width of 0.18mm and film thickness of 5-11 μm;
sixth step: respectively ultrasonically treating the substrate electrode in ethanol and deionized water for 3min, and drying at constant temperature of 50 ℃ in an oven;
seventh step: mixing the aged powder with ethanol reagent, and coating on a substrate electrode;
eighth step: aging in oven at 40deg.C for 24 hr.
As can be seen from FIG. 1, ni-SnO prepared by using urea as additive 2 Most of the materials are in a cubic form, are uniformly dispersed, have smooth surfaces, are broken in shells (shells of core-shell structures), are in lamellar structures, and have larger specific surface areas. This is because urea reacts in aqueous solution to form ammonia water and then ionizes to form hydroxide ions, which slowly releases OH as the reaction proceeds - Is favorable for the generation of uniform precipitation of the tin hydroxide
As can be seen from FIG. 2, ni-SnO 2 The lowest response operating temperature to formaldehyde is as low as 80 ℃. The optimum working temperature is 140 ℃. The doping of Ni effectively reduces contact potential and accelerates charge transfer, so that more oxygen vacancies are generated, the interaction between the adsorbed target gas and the metal oxide is promoted, and the gas sensitivity of tin dioxide is greatly improved.
From FIG. 3, it can be seen that Ni-SnO 2 The device has good response when the formaldehyde concentration is low, and the response of the device is gradually increased along with the increase of the concentration.
From FIG. 4, it can be seen that Ni-SnO 2 Response to formaldehyde and recovery time. At a formaldehyde concentration of 100ppm, the response time and recovery time were 91s and 26s, respectively.
As can be seen from fig. 5, Ni-SnO 2 The response sensitivity to different gases is far higher than that of other gases, and the formaldehyde gas has excellent gas-sensitive selectivity.
The foregoing description of the preferred embodiments of the invention should not be taken as limiting the scope of the invention, which is defined by the appended claims, but rather by the description of the preferred embodiments, all changes and modifications that come within the meaning and range of equivalency of the claims are intended to be embraced therein.
Claims (1)
1. Ni-SnO with urea as additive for low-power consumption formaldehyde detection 2 The preparation method of the gas-sensitive material is characterized by comprising the following steps:
the first step: weigh 8.75g SnCl 4 ·5H 2 O、0.59gNiCl 2 ·6H 2 Dissolving O and 2.65g of urea into 20mL of deionized water, stirring to completely dissolve, and performing ultrasonic treatment for 15min;
and a second step of: pouring the solution into a hydrothermal kettle, and reacting for 12 hours at the constant temperature of 180 ℃;
and a third step of: after cooling to room temperature, filtering and washing 3 times;
fourth step: aging in an oven to obtain white Ni-SnO 2 A powder;
fifth step: preparing silver-plated alumina ceramic electrodes, wherein the electrode spacing is 0.15mm, the electrode width is 0.18mm, and the film thickness is 5-11 mu m;
sixth step: respectively ultrasonically treating the alumina ceramic silver-plated electrode in ethanol and deionized water for 3min, and drying in a drying oven;
seventh step: mixing the aged powder obtained in the fourth step with an ethanol reagent, and coating the mixture on a silver-plated electrode of the substrate alumina ceramic;
eighth step: aging in an oven;
aging treatment is carried out for 24 hours at the constant temperature of 60 ℃;
in the sixth step, drying is carried out at a constant temperature of 50 ℃;
aging for 24 hours at the constant temperature of 40 ℃ in the eighth step;
urea as additivePrepared Ni-SnO 2 Most of the materials are in a cubic form, are uniformly dispersed, have smooth surfaces, are broken in the shell of the core-shell structure, are in a lamellar structure, and have a larger specific surface area;
Ni-SnO 2 the lowest response working temperature to formaldehyde is as low as 80 ℃, and the optimal working temperature is 140 ℃;
at a formaldehyde concentration of 100ppm, the response time and recovery time were 91s and 26s, respectively.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110727943.4A CN113447533B (en) | 2021-06-29 | 2021-06-29 | Ni-SnO with urea as additive for low-power consumption formaldehyde detection 2 Preparation method of gas-sensitive material |
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| CN113447533B true CN113447533B (en) | 2024-01-23 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107827150A (en) * | 2017-12-14 | 2018-03-23 | 上海交通大学 | A kind of nickel doped tin oxide nano material, formaldehyde gas sensor and preparation method |
| CN108828010A (en) * | 2018-08-22 | 2018-11-16 | 云南大学 | A kind of sensitive material detecting formaldehyde gas and preparation method and application |
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- 2021-06-29 CN CN202110727943.4A patent/CN113447533B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107827150A (en) * | 2017-12-14 | 2018-03-23 | 上海交通大学 | A kind of nickel doped tin oxide nano material, formaldehyde gas sensor and preparation method |
| CN108828010A (en) * | 2018-08-22 | 2018-11-16 | 云南大学 | A kind of sensitive material detecting formaldehyde gas and preparation method and application |
Non-Patent Citations (1)
| Title |
|---|
| The effect of Ni doping concentration on the gas sensing properties of Ni doped SnO2;Zhidong Lin et al.;Sensors and Actuators B: Chemical;501-510 * |
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