CN112479246A - Preparation of Ni-doped stannic oxide formaldehyde sensitive composite material based on ZIF-8 metal organic framework template, product and application - Google Patents
Preparation of Ni-doped stannic oxide formaldehyde sensitive composite material based on ZIF-8 metal organic framework template, product and application Download PDFInfo
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Abstract
The invention discloses a preparation method of a Ni-doped stannic oxide formaldehyde sensitive ternary composite material based on a ZIF-8 metal organic framework template, a product and an application thereof, wherein the method utilizes the ZIF-8 MOF material as a crystallization template, and thiourea is decomposed under the condition of glycol solvothermal to provide S2‑Generating SnS2And NiS precursor, and preparing Ni-doped SnO based on ZIF-8 metal organic framework template by regulating and controlling conditions such as roasting temperature, roasting time and the like of the precursor2A formaldehyde-sensitive ternary composite material. The ZIF-8 is taken as a template, so that the specific surface area of the prepared composite material can be greatly improved, and the Zn and Ni are doped, which is favorable for further improving the specific surface area of the prepared composite materialElevated SnO2Response value and selectivity to formaldehyde gas; the preparation method of the SnO prepared by the solvothermal method is simple, the reaction temperature is low, and the subsequent treatment is not needed2the/NiO @ ZIF-8 ternary composite material can be used for formaldehyde gas sensors and the like.
Description
Technical Field
The invention relates to a preparation technology of a metal oxide nano material, in particular to Ni-doped SnO based on a ZIF-8 metal organic framework template2A preparation method of a formaldehyde-sensitive ternary composite material, a product and application thereof.
Background
Formaldehyde is a carcinogenic gas, is commonly used in interior decoration materials, such as interlayer glue, paint, plastic products and the like of new furniture, and is one of main indoor pollution gases harmful to human bodies. The latest standard established by the world health organization is that the content of formaldehyde exposed to human bodies for a long time should not exceed 0.08 ppm. However, low concentrations of formaldehyde are difficult to detect by the human olfactory system. Therefore, the developed formaldehyde gas sensing material has a far-reaching practical significance on high formaldehyde sensitivity, strong anti-interference capability of other gases and stable chemical properties.
Tin dioxide is an n-type semiconductor with a wide forbidden band, and has an adjustable pore structure and a high specific surface area, so that defects are easily generated to dope impurities, and meanwhile, the tin dioxide is low in price, easy to synthesize, non-toxic and harmless, so that the tin dioxide nano-structure material is widely applied to sensitive materials of gas sensors. However, the gas-sensitive property of a single tin dioxide material is controlled by the morphology, crystal form, specific surface area, energy band structure and the like of the material, and the defects of low sensitivity to formaldehyde, poor selectivity and the like still exist.
Metal-Organic Framework (MOF) is a new type of porous material formed by Metal ions and Organic ligands through coordination bonds. The nano material obtained by taking the MOF as the template has the characteristics of high porosity and large specific surface area, and has more active chemical properties. At the same time due toThe presence of the ligand molecules can effectively prevent the doped metal elements from aggregating. Comparatively pure SnO2In terms of material, SnO2the/NiO composite material is easier to generate electron-hole exchange due to the difference of energy levels of a conduction band and a valence band, and has better selectivity to formaldehyde. So that SnO synthesized by taking ZIF-8 as template2the/NiO @ ZIF-8 ternary composite material has better gas-sensitive performance to formaldehyde. The invention takes ZIF-8 as a template and adopts a simple solvothermal method to prepare SnO2the/NiO @ ZIF-8 ternary composite nano material provides a high-quality gas-sensitive sensor material aiming at formaldehyde gas for the market.
Disclosure of Invention
The invention aims to provide Ni-doped SnO (SnO) based on ZIF-8 metal organic framework template2A preparation method of formaldehyde-sensitive ternary composite nano material.
Yet another object of the present invention is to: the Ni-doped SnO prepared by the method based on the ZIF-8 metal organic framework template is provided2Formaldehyde-sensitive ternary composite nano-material products.
Yet another object of the present invention is to: provides an application of the product.
The purpose of the invention is realized by the following scheme: a preparation method of a Ni-doped stannic oxide formaldehyde sensitive composite material based on a ZIF-8 metal organic framework template comprises the steps of using a ZIF-8 metal-organic framework Material (MOF) as a crystallization template, decomposing thiourea under the condition of glycol solvothermal to provide S2-, and generating SnS2And NiS precursor, and preparing Ni-doped SnO based on ZIF-8 metal organic framework template by regulating and controlling conditions such as roasting temperature, roasting time and the like of the precursor2The formaldehyde-sensitive ternary composite material comprises the following steps:
(1) pouring N-N Dimethylformamide (DMF) and methanol with the concentration of 2wt% into a flask according to the volume ratio of 1:2, and uniformly stirring;
(2) 0.8 to 1.0g of zinc nitrate hexahydrate (Zn (NO))3·6H2O) and 0.1-0.3 g of 2-methylimidazole (2-MI) are put into a flask and fully stirred at room temperature;
(3) transferring the solution in the flask to a beaker, completely reacting in an oven at 100 ℃, taking the precipitate, washing and drying to obtain ZIF-8 powder;
(4) 0.3g of dried ZIF-8 powder was put into 100mL of ethylene glycol ((CH)2OH)2) In the reaction solution, 0.1-0.2 g of nickel chloride hexahydrate (NiCl) is added simultaneously2·6H2O), 1.0 to 2.0g of stannous chloride dihydrate and 1.0 to 1.5g of thiourea (NH)2CSNH2) Or urea, and stirring uniformly;
(5) transferring the uniformly stirred solution into a polytetrafluoroethylene reaction kettle, reacting in an oven at 150-180 ℃ for 24 hours, taking the precipitate, washing and drying to obtain a precursor;
(6) putting the dried precursor into a crucible, putting the crucible into a muffle furnace, and roasting at 550-650 ℃ to obtain Ni-doped SnO based on a ZIF-8 metal organic framework template2A formaldehyde-sensitive ternary composite material.
The method has controllable Ni doping amount and uniform distribution of Ni and Zn elements, and provides a high-quality synthesis method of the gas-sensitive sensing material aiming at formaldehyde detection.
Wherein the volume of DMF in the step (1) is 40-50 mL, and the volume of methanol is 80-100 mL.
The rotating speed of the full stirring in the step (2) is 1000 revolutions per minute, and the stirring time is 20-30 min.
The reaction time in the step (3) is 20-24 h.
The thiourea described in step (4) may be replaced by an equimolar amount of urea.
In the step (6), the roasting speed is 3-5 ℃/min, and the roasting heat preservation time is 120-240 min.
The invention also provides Ni-doped SnO based on the ZIF-8 metal organic framework template2The formaldehyde-sensitive ternary composite material is prepared by any one of the methods.
In addition, the invention also provides Ni-doped SnO based on the ZIF-8 metal organic framework template2The formaldehyde-sensitive ternary composite material is applied to a formaldehyde gas sensor.
A simple and feasible preparation method of a Ni-doped SnO2 formaldehyde sensitive ternary composite material based on a ZIF-8 metal organic framework template is characterized in that a ZIF-8 MOF material is used as the template, stannous chloride, nickel chloride and thiourea are used as reactants to synthesize a precursor SnS2/NiS @ ZIF-8 by a solvothermal method, and then the precursor is simply roasted to synthesize the SnO2/NiO @ ZIF-8 ternary composite nanomaterial.
The invention takes ZIF-8 as a template and adopts a simple solvothermal method to prepare SnO2the/NiO @ ZIF-8 ternary composite nano material provides a high-quality gas-sensitive sensor material aiming at formaldehyde gas for the market. The specific surface area of the prepared composite material can be greatly improved by taking ZIF-8 as a template, and the doping of Zn and Ni is beneficial to further improving SnO2Response value and selectivity to formaldehyde gas; the preparation method of the SnO prepared by the solvothermal method is simple, the reaction temperature is low, and the subsequent treatment is not needed2the/NiO @ ZIF-8 ternary composite material can be used for formaldehyde gas sensors and the like.
The invention has the advantages that: the doping amount of Ni and Zn is controllable, the doping elements are uniformly distributed, and the ternary composite nano material has high purity, uniform size, sensitivity and selectivity to formaldehyde and pure SnO2Compared with the nanometer material, the nanometer material is greatly improved.
Drawings
FIG. 1 is SnO of example 1 of the present invention2The real-time response curve of the/NiO @ ZIF-8 ternary composite nano material to 200ppm formaldehyde gas;
FIG. 2 is SnO of example 2 of the present invention2The response value of the/NiO @ ZIF-8 ternary composite nano material to different gases of 200ppm of formaldehyde, methanol, ethanol, acetone and ammonia gas.
Detailed Description
Example 1:
a ZIF-8 metal-organic framework template-based Ni-doped stannic oxide formaldehyde sensitive composite material is prepared by taking a ZIF-8 metal-organic framework material as a crystallization template, decomposing thiourea under the solvothermal condition of ethylene glycol to provide S2-, and generating SnS2And NiS precursor, and roasting the precursor by regulating and controllingPreparing Ni-doped SnO based on ZIF-8 metal organic framework template at temperature and roasting time2The formaldehyde-sensitive ternary composite material is prepared by the following steps:
(1) weighing 50mL of N-N Dimethylformamide (DMF) and 100mL of methanol with the concentration of 2wt% and pouring into a flask, and uniformly stirring;
(2) 0.8g of zinc nitrate hexahydrate (Zn (NO)3·6H2O) and 0.1g of 2-methylimidazole (2-MI) were placed in a flask and sufficiently stirred at room temperature;
(3) transferring the solution in the flask to a beaker, completely reacting in an oven at 100 ℃, taking the precipitate, washing and drying to obtain ZIF-8 powder;
(4) 0.3g of dried ZIF-8 powder was put into 100mL of ethylene glycol ((CH)2OH)2) In (1), 0.1g of nickel chloride hexahydrate (NiCl) was added simultaneously2·6H2O), 1.0g stannous chloride dihydrate and 1.1g thiourea (NH)2CSNH2) Stirring uniformly;
(5) transferring the uniformly stirred solution into a polytetrafluoroethylene reaction kettle, reacting in an oven at 150 ℃ for 24 hours, taking the precipitate, washing and drying to obtain a precursor;
(6) putting the dried precursor into a crucible, putting the crucible into a muffle furnace, and roasting the precursor for 2 hours at 550 ℃ to obtain Ni-doped SnO based on a ZIF-8 metal organic framework template2A formaldehyde-sensitive ternary composite material.
FIG. 1 is the SnO2And a real-time response curve of the gas-sensitive sensing device made of the/NiO @ ZIF-8 ternary composite nano material to 200ppm of formaldehyde gas at 230 ℃. It can be seen that the material produces very high response values to formaldehyde.
Example 2:
an Ni-doped stannic oxide formaldehyde sensitive composite material based on a ZIF-8 metal organic framework template is similar to that in the embodiment 1, and is prepared by the following steps:
(1) 30mL of N-N Dimethylformamide (DMF) and 60mL of methanol with the concentration of 2wt% are weighed and poured into a flask, and the mixture is uniformly stirred;
(2) 0.9g of zinc nitrate hexahydrate (Zn (NO)3·6H2O) and 0.2g2-methylimidazole (2-MI) is put into a flask and fully stirred at room temperature;
(3) transferring the solution in the flask to a beaker, completely reacting in an oven at 100 ℃, taking the precipitate, washing and drying to obtain ZIF-8 powder;
(4) 0.3g of dried ZIF-8 powder was put into 100mL of ethylene glycol ((CH)2OH)2) In (1), 0.15g of nickel chloride hexahydrate (NiCl) was added simultaneously2·6H2O), 1.5g stannous chloride dihydrate and 1.3g thiourea (NH)2CSNH2) Stirring uniformly;
(5) transferring the uniformly stirred solution into a polytetrafluoroethylene reaction kettle, reacting for 24 hours in an oven at 160 ℃, taking the precipitate, washing and drying to obtain a precursor;
(6) putting the dried precursor into a crucible, putting the crucible into a muffle furnace, and roasting the precursor for 2 hours at 600 ℃ to obtain Ni-doped SnO based on a ZIF-8 metal organic framework template2A formaldehyde-sensitive ternary composite material.
FIG. 2 is the SnO2And a response value histogram of a sensing device made of the/NiO @ ZIF-8 ternary composite nano material to various gases of 200ppm of formaldehyde, methanol, ethanol, acetone and ammonia gas at 230 ℃. The response value of the material to formaldehyde is far higher than that of other gases, which shows that the material has good selectivity and can effectively avoid the interference of other gases to the detection result.
Example 3:
an Ni-doped stannic oxide formaldehyde sensitive composite material based on a ZIF-8 metal organic framework template is similar to that in the embodiment 1, and is prepared by the following steps:
(1) weighing 40mL of N-N Dimethylformamide (DMF) and 80mL of methanol with the concentration of 2wt%, pouring into a flask, and uniformly stirring;
(2) 1.0g of zinc nitrate hexahydrate (Zn (NO)3·6H2O) and 0.3g of 2-methylimidazole (2-MI) were placed in a flask and sufficiently stirred at room temperature;
(3) transferring the solution in the flask to a beaker, completely reacting in an oven at 100 ℃, taking the precipitate, washing and drying to obtain ZIF-8 powder;
(4) 0.3g of dried ZIF-8 powder was put into 100mL of ethylene glycol ((CH)2OH)2) In (1), 0.2g of nickel chloride hexahydrate (NiCl) was added simultaneously2·6H2O), 2.0g stannous chloride dihydrate and 1.5g thiourea (NH)2CSNH2) Stirring uniformly;
(5) transferring the uniformly stirred solution into a polytetrafluoroethylene reaction kettle, reacting in an oven at 180 ℃ for 24 hours, taking the precipitate, washing and drying to obtain a precursor;
(6) putting the dried precursor into a crucible, putting the crucible into a muffle furnace, and roasting the crucible at 650 ℃ for 2 hours to obtain Ni-doped SnO based on a ZIF-8 metal organic framework template2A formaldehyde-sensitive ternary composite material.
Claims (7)
1. A preparation method of a Ni-doped stannic oxide formaldehyde sensitive composite material based on a ZIF-8 metal-organic framework template is characterized in that a ZIF-8 metal-organic framework material is used as a crystallization template, thiourea is decomposed under the condition of glycol solvothermal to provide S2-, and SnS is generated2And NiS precursor, and preparing Ni-doped SnO based on ZIF-8 metal organic framework template by regulating and controlling the roasting temperature and roasting time of the precursor2The formaldehyde-sensitive ternary composite material comprises the following steps:
(1) pouring N-N Dimethylformamide (DMF) and methanol with the concentration of 2wt% into a flask according to the volume ratio of 1:2, and uniformly stirring;
(2) 0.8 to 1.0g of zinc nitrate hexahydrate (Zn (NO))3·6H2O) and 0.1-0.3 g of 2-methylimidazole (2-MI) are put into a flask and fully stirred at room temperature;
(3) transferring the solution in the flask to a beaker, completely reacting in an oven at 100 ℃, taking the precipitate, washing and drying to obtain ZIF-8 powder;
(4) 0.3g of dried ZIF-8 powder was put into 100mL of ethylene glycol ((CH)2OH)2) In the reaction solution, 0.1-0.2 g of nickel chloride hexahydrate (NiCl) is added simultaneously2·6H2O), 1.0 to 2.0g of stannous chloride dihydrate and 1.0 to 1.5g of thiourea (NH)2CSNH2) Or urea, and stirring uniformly;
(5) transferring the uniformly stirred solution into a polytetrafluoroethylene reaction kettle, reacting in an oven at 150-180 ℃ for 24 hours, taking the precipitate, washing and drying to obtain a precursor;
(6) putting the dried precursor into a crucible, putting the crucible into a muffle furnace, and roasting at 550-650 ℃ to obtain Ni-doped SnO based on a ZIF-8 metal organic framework template2A formaldehyde-sensitive ternary composite material.
2. The method of claim 1, wherein: in the step (1), the volume of DMF is 40-50 mL, and the volume of methanol is 80-100 mL.
3. The method of claim 1, wherein: in the step (2), the rotation speed of the full stirring is 1000 revolutions per minute, and the stirring time is 20-30 min.
4. The method of claim 1, wherein: in the step (3), the reaction time is 20-24 h.
5. The method of claim 1, wherein: in the step (6), the temperature rising speed of the roasting is 3-5 ℃/min, and the heat preservation time of the roasting is 120-240 min.
6. Ni-doped SnO based on ZIF-8 metal organic framework template2A formaldehyde-sensitive composite material, characterized in that it is prepared according to any one of claims 1 to 6.
7. The ZIF-8 metal organic framework template-based Ni-doped SnO according to claim 62The formaldehyde sensitive composite material is applied as a gas sensor material.
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| CN114059096A (en) * | 2021-12-17 | 2022-02-18 | 北京化工大学 | Preparation of nickel-doped tin dioxide catalyst and application of nickel-doped tin dioxide catalyst in electrocatalysis |
| CN114772561A (en) * | 2022-05-07 | 2022-07-22 | 合肥工业大学 | Hollow multi-shell Sn-containing metal selenide @ carbon heterojunction and application thereof |
| CN115326889A (en) * | 2022-08-08 | 2022-11-11 | 吉林大学 | Xylene gas sensor based on core-shell mesoporous Sn doped NiO sensitive material derived from MOF and preparation method thereof |
| CN115849435A (en) * | 2022-12-26 | 2023-03-28 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of tin dioxide nano material for gas detection, product and application thereof |
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