CN113447533A - Ni-SnO with urea as additive for low-power-consumption formaldehyde detection2Preparation method of gas-sensitive material - Google Patents
Ni-SnO with urea as additive for low-power-consumption formaldehyde detection2Preparation method of gas-sensitive material Download PDFInfo
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- CN113447533A CN113447533A CN202110727943.4A CN202110727943A CN113447533A CN 113447533 A CN113447533 A CN 113447533A CN 202110727943 A CN202110727943 A CN 202110727943A CN 113447533 A CN113447533 A CN 113447533A
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- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 title claims abstract description 83
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 239000004202 carbamide Substances 0.000 title claims abstract description 25
- 239000000463 material Substances 0.000 title claims abstract description 17
- 239000000654 additive Substances 0.000 title claims abstract description 16
- 230000000996 additive effect Effects 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 230000032683 aging Effects 0.000 claims abstract description 13
- 238000001514 detection method Methods 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 239000000758 substrate Substances 0.000 claims abstract description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 230000002431 foraging effect Effects 0.000 claims abstract description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 4
- 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
- 238000007747 plating Methods 0.000 claims abstract description 4
- 229910052709 silver Inorganic materials 0.000 claims abstract description 4
- 239000004332 silver 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
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 18
- 229910001868 water Inorganic materials 0.000 claims description 3
- 230000004044 response Effects 0.000 abstract description 7
- 238000011084 recovery Methods 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 abstract 1
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 abstract 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 abstract 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 28
- 230000035945 sensitivity Effects 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 3
- 229910000069 nitrogen hydride 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
- 206010028980 Neoplasm Diseases 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 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
- 201000011510 cancer Diseases 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
- 239000011258 core-shell material Substances 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 hydroxyl 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
- 210000004379 membrane Anatomy 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 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
- 229910000510 noble metal Inorganic materials 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
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001737 promoting effect 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
- 238000012546 transfer Methods 0.000 description 1
Images
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
-
- 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 detection2A preparation method of a gas-sensitive material belongs to the technical field of formaldehyde detection, and comprises the following steps: weighing SnCl4·5H2O、NiCl2·6H2Stirring O and urea in deionized water to completely dissolve the O and the urea; pouring the solution into a hydrothermal kettle, and reacting at constant temperature; cooling to room temperature, filtering and washing; putting the mixture into an oven for aging; plating silver electrodes on the alumina ceramic, wherein the electrode distance is 0.15mm, the electrode width is 0.18mm, and the film thickness is 5-11 mu m; respectively carrying out ultrasonic treatment on the substrate electrode in ethanol and deionized water for 3min, and drying; aging the powder, mixing the powder with an ethanol reagent, and coating the mixture on a substrate electrode; aging in an oven. The invention can obtain uniform Ni-SnO with large specific surface area by using the urea additive with lower cost2The gas-sensitive material and the prepared formaldehyde gas-sensitive device have the advantages of low working temperature, low energy consumption, short response and recovery time and high sensitivityGood selectivity and good stability.
Description
Technical Field
The invention belongs to the technical field of formaldehyde detection, and particularly relates to Ni-SnO with urea as an additive for low-power-consumption formaldehyde detection2A preparation method of the 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 life, needs to be paid particular attention. Formaldehyde is classified as a serious carcinogen by the international agency for research on cancer. Formaldehyde has a strong irritating effect on the skin and body mucous membranes (such as nose, voice and eye membranes) and even coagulates and denatures human proteins.
At present, target gas monitoring mainly comprises a gas chromatography, an infrared spectroscopy, a photoacoustic spectrometry 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 high sensitivity to various combustible gases, industrial waste gases, polluted gases and other gases is often used for manufacturing gas sensors.
However, the sensitivity and selectivity of pure tin dioxide materials to formaldehyde are not ideal. However, the noble metal modified tin dioxide can improve the gas-sensitive performance of the tin oxide gas-sensitive material, but causes the problems of sharply increased cost, environmental pollution and the like. In summary, the existing semiconductor gas-sensitive sensor has the defects of high working temperature, high energy consumption and the like, and the gas sensing material with high sensitivity to formaldehyde, good selectivity and low cost at lower working temperature is continuously and further developed.
Disclosure of Invention
The invention aims to solve the existing problems and provides Ni-SnO (nickel-stannic oxide) taking urea as an additive for low-power-consumption formaldehyde detection2A preparation method of the gas sensitive material.
The invention is realized by the following technical scheme:
Ni-SnO with urea as additive for low-power-consumption formaldehyde detection2The preparation method of the gas sensitive material comprises the following steps:
the first step is as follows: 8.75g SnCl was weighed4·5H2O、0.59gNiCl2·6H2Dissolving O and 2.65g of urea into 20ml of deionized water, stirring to completely dissolve the O and the urea, and performing ultrasonic treatment for 15 min;
the second step is that: pouring the solution into a hydrothermal kettle, and reacting for 12 hours at the constant temperature of 180 ℃;
the third step: after cooling to room temperature, filtration and washing 3 times;
the fourth step: putting the mixture into an oven for aging to obtain white SnO2(NH3·H2O) powder;
the fifth step: plating silver electrodes on the alumina ceramic, wherein the electrode distance is 0.15mm, the electrode width is 0.18mm, and the film thickness is 5-11 mu m;
and a sixth step: respectively carrying out ultrasonic treatment on the substrate electrode in ethanol and deionized water for 3min, and drying in an oven;
the seventh step: aging the powder, mixing the powder with an ethanol reagent, and coating the mixture 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 constant temperature 60 ℃ aging for 24 h.
Further, the drying in the sixth step is constant temperature of 50 ℃.
And further, the aging in the eight steps is aging for 24 hours at the constant temperature of 40 ℃.
Compared with the prior art, the invention has the following advantages:
by adopting the scheme, the urea for low-power-consumption formaldehyde detection is used as Ni-SnO of the additive2The 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 the urea additive with lower cost2The 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 source, low price, operation and control of the process, high yield and easy realization of industrial production and application.
Drawings
FIG. 1 shows the preparation of Ni-SnO by hydrothermal method using urea as additive in this application2SEM images of the samples;
FIG. 2 shows Ni-SnO at different working temperatures in the present application2Formaldehyde poisoning effectThe preparation method comprises the following steps of;
FIG. 3 shows Ni-SnO in the present application2Response characteristics at different concentrations of formaldehyde;
FIG. 4 shows Ni-SnO in the present application2Response to formaldehyde and recovery time;
FIG. 5 shows Ni-SnO in the present application2Selectivity to formaldehyde gas.
Detailed Description
Ni-SnO with urea as additive for low-power-consumption formaldehyde detection2The preparation method of the gas sensitive material comprises the following steps:
the first step is as follows: 8.75g SnCl was weighed4·5H2O、0.59gNiCl2·6H2Dissolving O and 2.65g of urea into 20ml of deionized water, stirring to completely dissolve the O and the urea, and performing ultrasonic treatment for 15 min;
the second step is that: pouring the solution into a hydrothermal kettle, and reacting for 12 hours at the constant temperature of 180 ℃;
the third step: after cooling to room temperature, filtration and washing 3 times;
the fourth step: placing the mixture into an oven for aging for 24 hours at the constant temperature of 60 ℃ to obtain white SnO2(NH3·H2O) powder;
the fifth step: plating silver electrodes on the alumina ceramic, wherein the electrode distance is 0.15mm, the electrode width is 0.18mm, and the film thickness is 5-11 mu m;
and a sixth step: respectively carrying out ultrasonic treatment on the substrate electrode in ethanol and deionized water for 3min, and drying in an oven at constant temperature of 50 ℃;
the seventh step: aging the powder, mixing the powder with an ethanol reagent, and coating the mixture on a substrate electrode;
eighth step: placing the mixture into an oven to age for 24 hours under the constant temperature condition of 40 ℃.
As can be seen from FIG. 1, Ni-SnO prepared by using urea as additive2Most of the materials are in a cubic form, are uniformly dispersed, have smooth surfaces, are broken (shells of core-shell structures), have lamellar structures inside and have larger specific surface area. The reason is that the urea reacts in the aqueous solution to generate ammonia water, then is ionized to generate hydroxyl ions, and OH is slowly released along with the reaction-Is favorable to the homogeneity of tin hydroxideFormation of a homogeneous precipitate
From FIG. 2, it can be seen that Ni-SnO2The lowest response to formaldehyde operating temperature is as low as 80 ℃. The optimal working temperature is 140 ℃. And the doping of Ni effectively reduces the contact potential, accelerates the charge transfer, thereby generating more oxygen vacancies, promoting the interaction between the adsorbed target gas and the metal oxide, and greatly improving the gas-sensitive performance of the tin dioxide.
From FIG. 3, Ni-SnO can be seen2The formaldehyde concentration is low, the response is good, 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-SnO2Response 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-SnO2The response sensitivity to different gases is far higher than that of other gases, and the gas sensitive selectivity to formaldehyde gas is excellent.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention, and the present invention is not limited to the illustrated embodiments, and all the modifications and equivalents of the embodiments may be made without departing from the spirit of the present invention.
Claims (4)
1. Ni-SnO with urea as additive for low-power-consumption formaldehyde detection2The preparation method of the gas-sensitive material is characterized by comprising the following steps of:
the first step is as follows: 8.75g SnCl was weighed4·5H2O、0.59gNiCl2·6H2Dissolving O and 2.65g of urea into 20ml of deionized water, stirring to completely dissolve the O and the urea, and performing ultrasonic treatment for 15 min;
the second step is that: pouring the solution into a hydrothermal kettle, and reacting for 12 hours at the constant temperature of 180 ℃;
the third step: after cooling to room temperature, filtration and washing 3 times;
the fourth step: putting the mixture into an oven for aging to obtain white SnO2(NH3·H2O) powder;
the fifth step: plating silver electrodes on the alumina ceramic, wherein the electrode distance is 0.15mm, the electrode width is 0.18mm, and the film thickness is 5-11 mu m;
and a sixth step: respectively carrying out ultrasonic treatment on the substrate electrode in ethanol and deionized water for 3min, and drying in an oven;
the seventh step: aging the powder, mixing the powder with an ethanol reagent, and coating the mixture on a substrate electrode;
eighth step: and (5) putting the mixture into an oven for aging.
2. The Ni-SnO with urea as an additive for low-power formaldehyde detection according to claim 12The preparation method of the gas sensitive material is characterized in that the aging treatment in the fourth step is constant temperature aging at 60 ℃ for 24 h.
3. The Ni-SnO with urea as an additive for low-power formaldehyde detection according to claim 12The preparation method of the gas sensitive material is characterized in that the drying in the sixth step is constant temperature of 50 ℃.
4. The Ni-SnO with urea as an additive for low-power formaldehyde detection according to claim 12The preparation method of the gas sensitive material is characterized in that the aging in the eighth step is aging for 24 hours at a constant temperature of 40 ℃.
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|---|---|---|---|
| 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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| 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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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 |
|---|
| ZHIDONG LIN ET AL.: "The effect of Ni doping concentration on the gas sensing properties of Ni doped SnO2", SENSORS AND ACTUATORS B: CHEMICAL * |
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