CN114988457A - Based on alpha-Fe 2 O 3 Nanowire heteroepitaxy ZnO @ ZIF-8 microporous nanomaterial, and preparation process and application thereof - Google Patents
Based on alpha-Fe 2 O 3 Nanowire heteroepitaxy ZnO @ ZIF-8 microporous nanomaterial, and preparation process and application thereof Download PDFInfo
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Abstract
The invention discloses a method based on alpha-Fe 2 O 3 A microporous nano material of nanowire heteroepitaxy ZnO @ ZIF-8, a preparation process and application. The invention adopts a thermal oxidation method to prepare alpha-Fe 2 O 3 Heteroepitaxy ZnO as seed crystal layer by atomic layer deposition technology, further epitaxy MOF material ZIF-8 by solvothermal technology to obtain alpha-Fe 2 O 3 Nanowire heteroepitaxy ZnO @ ZIF-8 microporous nanomaterial. The method has the advantages of good repeatability, high yield, high preparation efficiency, large-scale production and the like, and provides a brand new idea for large-scale preparation of heterogeneous MOSs @ MOF gas-sensitive nano materials. The prepared MOF-based heterogeneous microporous nanowire gas sensing device can be used for sensing sulfurThe hydrogen hydride gas realizes ultra-sensitive, high-precision and high-selectivity detection, and has wide application prospect in the fields of environmental monitoring, medical health, food safety detection and the like.
Description
Technical Field
The invention relates to the technical field of semiconductor nano material preparation and gas sensing application, in particular to a method based on alpha-Fe 2 O 3 A microporous nano material of nanowire heteroepitaxy ZnO @ ZIF-8, a preparation process and application.
Background
Hydrogen sulfide is an acidic harmful corrosive gas generated in the production processes of natural gas purification, petroleum refining, sewage treatment, synthetic rayon, gas production, pharmacy, paper making and the like, and in the process of organic matter putrefaction. The hydrogen sulfide is unstable in chemical property, explosion can occur when the hydrogen sulfide is mixed with air for combustion, and leakage can cause serious environmental pollution. In addition, hydrogen sulfide can cause great harm to human health. The hydrogen sulfide is a strong neurotoxic substance, has obvious stimulation effect on mucous membrane, and can cause eye stabbing pain, lacrimation, vomiting, even pneumonia and pulmonary edema when the concentration is lower; and when high-concentration hydrogen sulfide is inhaled, olfactory nerves of a human body can be paralyzed, so that consciousness is suddenly lost, and even coma and asphyxia are caused to death. Therefore, the development of a hydrogen sulfide gas sensor with high sensitivity, quick response and good stability has great significance in real-time monitoring of the concentration of hydrogen sulfide in the environment. With the continuous development of modern medicine, the hydrogen sulfide gas sensor with high precision and high selectivity can be widely applied to the field of exhaled breath disease detection, for example, related literature reports that the concentration of hydrogen sulfide in exhaled breath of a human body can be efficiently screened in a noninvasive mode for diseases such as asthma and Chronic Obstructive Pulmonary Disease (COPD) and the like. In addition, part of food in life can generate special gas with the smell of rotten eggs in the deterioration process, so the hydrogen sulfide gas sensor also has great application prospect in the field of food safety.
In recent years, various types of gas sensors including electrochemical type and chemical resistance type have been widely used for sensing hydrogen sulfide gas in various fields. Among them, the semiconductor chemical resistance type has received important research attention due to its advantages of high sensitivity, simple device structure, low cost, etc. The development of efficient gas-sensitive materials is crucial to the preparation of high-performance chemiresistor-type gas sensors.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a catalyst based on alpha-Fe 2 O 3 A microporous nano material of nanowire heteroepitaxy ZnO @ ZIF-8, a preparation process and application. The invention provides a novel efficient large-scale preparation method of alpha-Fe 2 O 3 Nanowire and method of manufacturing the sameThe specific scheme of the synthetic route of the heteroepitaxial ZnO @ ZIF-8 microporous nano material is that firstly, the nuclear layer alpha-Fe is prepared by a thermal oxidation method with simple process 2 O 3 Carrying out heteroepitaxy on ZnO serving as a seed crystal layer by virtue of an atomic layer deposition technology, further carrying out epitaxy on an MOF material ZIF-8 by virtue of a solvothermal process, and finally obtaining alpha-Fe 2 O 3 The nanowire hetero-epitaxy ZnO @ ZIF-8 microporous nanomaterial is disclosed. The method adopts an advanced atomic layer deposition technology and a simple solvothermal method, has the advantages of good repeatability, high yield, high preparation efficiency, large-scale production and the like, and provides a brand new thought for large-scale preparation of the novel heterogeneous MOS @ MOF gas-sensitive nano material. The MOF-based heterogeneous microporous nanowire gas-sensitive material prepared by the method has the characteristics of high porosity, large specific surface area, high thermal stability and the like, and can realize ultrasensitive, high-precision and high-selectivity detection on ppb level trace hydrogen sulfide gas.
In the present invention, the nuclear layer is alpha-Fe 2 O 3 The preparation of the nano-wire adopts a thermal oxidation method, heteroepitaxy ZnO is used as a seed crystal layer by means of an atomic layer deposition technology, and a final product, namely alpha-Fe, is obtained by further epitaxy ZIF-8 through a solvothermal technology 2 O 3 The nanowire hetero-epitaxy ZnO @ ZIF-8 microporous nanomaterial is disclosed. The technical solution of the present invention is as follows.
The invention provides a catalyst based on alpha-Fe 2 O 3 The preparation process of the nanowire heteroepitaxy ZnO @ ZIF-8 microporous nanomaterial comprises the following specific steps:
(1) the foamed iron which is cleaned by ultrasonic and dried fully is used as a substrate and a source material, and is put into a muffle furnace for thermal oxidation to obtain alpha-Fe 2 O 3 A nanowire;
(2) the alpha-Fe growing in the step (1) 2 O 3 Placing the foamed iron substrate of the nanowire into an atomic layer deposition system to deposit a ZnO film and provide a seed crystal layer for the subsequent growth of ZIF-8;
(3) reversing the sample prepared by atomic layer deposition in the step (2) into a hydrothermal kettle, epitaxially growing a ZIF-8 nano structure by a solvothermal method, and flushing with absolute ethyl alcohol after the reaction is finishedWashing and drying to obtain alpha-Fe 2 O 3 Nanowire heteroepitaxy ZnO @ ZIF-8 microporous nanomaterial.
In the step (1), the ultrasonic cleaning specifically comprises sequentially performing ultrasonic cleaning for 10-15 min by using absolute ethyl alcohol and deionized water respectively.
In the step (1), the atmosphere of the muffle furnace thermal oxidation process is air, the growth temperature is 600-800 ℃, and the growth time is 6-12 hours.
alpha-Fe obtained in the step (1) 2 O 3 The average diameter of the nanowires is 60-110 nm, and the average length of the nanowires is 10-15 mu m.
In the step (2), the specific process of atomic layer deposition is to select DEZ (diethyl zinc) as a zinc source, deionized water as an oxygen source, set the reaction temperature to be 150-220 ℃, and finally set the growth rate of the ZnO film to be 0.20-0.30 nm/cycle.
In the step (2), the thickness of the atomic layer deposition ZnO film is 5-50 nm.
In the step (3), the solvent for solvothermal growth is DMF/H with the volume ratio of 3:1 2 And the precursor of the O solution is 2-methylimidazole, the concentration of the precursor solution is 0.05-0.4 mol/L, the growth temperature is 60-80 ℃, and the growth time is 5-10 hours.
The invention also provides alpha-Fe-based material prepared by the preparation process 2 O 3 Nanowire heteroepitaxy ZnO @ ZIF-8 microporous nanomaterial. alpha-Fe obtained by the invention 2 O 3 The average diameter of the heteroepitaxial ZnO @ ZIF-8 microporous nanowire is 70-400 nm, the average length is 10-15 mu m, and the average pore size of the micropores is 0.3-0.4 nm.
The invention further provides a catalyst based on alpha-Fe 2 O 3 The application of the nano-wire heteroepitaxy ZnO @ ZIF-8 microporous nano material in the aspect of hydrogen sulfide gas sensing. alpha-Fe obtained by the invention 2 O 3 The nano-wire heteroepitaxy ZnO @ ZIF-8 microporous nano material can detect hydrogen sulfide gas of 0.05-50 ppm, and can be widely applied to the fields of environmental monitoring, human body exhaled breath disease detection and analysis, gas leakage monitoring, food safety detection and the like.
Compared with the prior art, the invention has the beneficial effects that:
1. compared with other single metal oxide core-shell heterogeneous nano materials, the invention is applied to alpha-Fe 2 O 3 Based on the @ ZnO core-shell nano material, an MOF material ZIF-8 is further subjected to hydrothermal epitaxy, and the ZIF-8 is a porous crystal material formed by a novel metal-organic framework, so that on one hand, the porosity and the specific surface area of the material can be effectively increased, the adsorption and response capability of the material to gas can be greatly improved, and meanwhile, the response time and the recovery time can be effectively shortened; on the other hand, the regular pores can effectively block gas molecules with the size larger than that of the pores, so that the selectivity of the material is greatly improved, and the problem of poor selectivity of the pure MOS material is effectively solved.
2. Compared with other homogeneous metal oxide @ MOF materials, the combined atomic layer deposition technology realizes the heteroepitaxy of the MOF material, namely, the heteroepitaxy is carried out on alpha-Fe 2 O 3 Hetero-epitaxial growth of ZnO @ ZIF-8 microporous nano material, alpha-Fe, on nano line 2 O 3 The presence of the heterojunction with ZnO can further improve the gas-sensitive response of the material.
3. According to the invention, heteroepitaxy of the ZIF-8 material is realized by depositing the ZnO seed crystal layer through the atomic layer, and the atomic layer deposition process can realize uniform coating of the heterogeneous seed crystal layer on the nanowire material with a high depth-to-width ratio, and has the advantages of good consistency and repeatability, high preparation efficiency, suitability for large-scale preparation and the like.
4. alpha-Fe of the invention 2 O 3 The nanowire heteroepitaxy ZnO @ ZIF-8 microporous nano gas-sensitive material can be used for detecting 0.05-50 ppm trace H 2 S realizes ultra-sensitive and high-selectivity detection, and can be widely applied to the fields of environmental monitoring, human body exhaled breath disease analysis, gas leakage monitoring, food safety detection and the like.
Drawings
FIG. 1 shows that the invention is based on alpha-Fe 2 O 3 A flow block diagram of a preparation process of a nanowire heteroepitaxy ZnO @ ZIF-8 microporous nanomaterial.
FIG. 2 shows α -Fe obtained in example 1 2 O 3 Heteroepitaxy of nanowiresSEM representation picture of ZnO @ ZIF-8 microporous nano material.
FIG. 3 shows α -Fe obtained in example 1 2 O 3 TEM representation picture of nano-wire heteroepitaxy ZnO @ ZIF-8 microporous nano-material.
FIG. 4 shows pure α -Fe obtained in example 1 2 O 3 Nanowire, alpha-Fe 2 O 3 @ ZnO core-shell nanowire and alpha-Fe 2 O 3 Micro H of @ ZnO @ ZIF-8 heterogeneous microporous nanowire 2 S gas-sensitive performance test result chart.
FIG. 5 shows α -Fe obtained in example 1 2 O 3 Nanowire heteroepitaxy ZnO @ ZIF-8 microporous nanomaterial-based gas sensing device for seven common gases (H) 2 S、NH 3 Acetone, ethanol, methane, CO and NO 2 ) Selective gas sensitive test result graph of (1).
FIG. 6 shows α -Fe obtained in example 2 2 O 3 SEM representation of the nano-material of the nano-wire heteroepitaxy ZnO @ ZIF-8.
FIG. 7 shows α -Fe obtained in example 2 2 O 3 Trace H of nano-wire heteroepitaxy ZnO @ ZIF-8 microporous nano-material-based gas sensing device 2 S gas-sensitive performance test result chart.
Detailed Description
The invention is described in further detail below with reference to the figures and examples.
The invention relates to a method based on alpha-Fe 2 O 3 The flow block diagram of the preparation process of the nanowire heteroepitaxy ZnO @ ZIF-8 microporous nanomaterial is shown in figure 1.
Example 1
(1) Ultrasonically cleaning absolute ethyl alcohol and deionized water for 10 min respectively, taking fully dried foam iron (1 cm x 1 cm) as a substrate and a source material, putting the substrate and the source material into a muffle furnace for thermal oxidation at the growth temperature of 600 ℃ for 12 hours to obtain alpha-Fe 2 O 3 The average diameter of the nanowires is about 70 nm, and the average length of the nanowires is more than 10 mu m;
(2) the alpha-Fe growing in the step (1) 2 O 3 Foam iron lining of nano wireDepositing a ZnO film in an atomic layer deposition system at the bottom to provide a seed crystal layer for the subsequent growth of ZIF-8, wherein DEZ (diethyl zinc) is selected as a zinc source, deionized water is selected as an oxygen source, the reaction temperature is set to be 200 ℃, the number of growth cycles is set to be 125 cycles, and alpha-Fe is prepared 2 O 3 The nanowire hetero-epitaxial ZnO thin film material is characterized in that the thickness of a ZnO shell layer thin film is 25 nm;
(3) 0.2 g of 2-methylimidazole are dissolved in 16 ml of DMF/H in a volume ratio of 3:1 2 The O solvent is used as a precursor solution of solvent thermal reaction and poured into a 30 ml hydrothermal kettle;
(4) reversing the sample prepared by atomic layer deposition in the step (2) into a hydrothermal kettle, putting the hydrothermal kettle into an oven for reacting for 8 hours at 70 ℃, naturally cooling the sample to room temperature after the reaction is finished, washing the sample with absolute ethyl alcohol and drying the sample to obtain alpha-Fe 2 O 3 SEM (scanning electron microscope) images and TEM (transmission electron microscope) images of the nano-wire heteroepitaxy ZnO @ ZIF-8 microporous nanomaterial are shown in figures 2 and 3, and thus the microporous nanomaterial ZIF-8 is uniformly coated on the alpha-Fe 2 O 3 @ ZnO nanowire surface, and α -Fe 2 O 3 The average diameter of the heteroepitaxial ZnO @ ZIF-8 microporous nanowire is about 320 nm, the average length is more than 10 mu m, and the average pore size of the micropores is 0.34 nm.
In the examples, the pure alpha-Fe obtained was used separately 2 O 3 Nanowire of alpha-Fe 2 O 3 @ ZnO core-shell nanowire and alpha-Fe 2 O 3 @ ZnO @ ZIF-8 heterogeneous microporous nanowire for H of 0.2-10 ppm 2 And carrying out gas sensing test on the S gas.
As shown in fig. 4, the test results are as follows: for 10 ppm of H 2 S gas, alpha-Fe 2 O 3 The response value (defined as R) of the @ ZnO @ ZIF-8 heterogeneous microporous nanowire a /R g Wherein R is a Is resistance in air, R g Is the resistance in the gas to be measured) is 32.2, and pure alpha-Fe 2 O 3 The response value of the nanowire is 2.4, alpha-Fe 2 O 3 The response value of the @ ZnO core-shell nanowire is 20.5, and the result shows that the alpha-Fe nanowire provided by the invention 2 O 3 Nanowire heteroepitaxy ZnO @ ZIF-8 microporous nano gas-sensitive material pair 10 ppm of H 2 Sensing response of S gas compared to pure alpha-Fe 2 O 3 The nano wire is improved by more than 12 times compared with alpha-Fe 2 O 3 The @ ZnO core-shell nanowire is also obviously improved. Meanwhile, the test results show that the alpha-Fe of the invention 2 O 3 Nanowire heteroepitaxy ZnO @ ZIF-8 microporous nano gas-sensitive material pair H 2 The detection limit of S gas is at least as low as ppb level, and H can be detected 2 And (4) detecting trace amount of S gas.
Furthermore, for the obtained alpha-Fe 2 O 3 The nanometer line heteroepitaxy ZnO @ ZIF-8 micropore nanometer material is subjected to selectivity test, namely H with the same concentration (10 ppm) is respectively subjected to selectivity test 2 S、NH 3 Acetone, ethanol, methane, CO and NO 2 A gas sensing test was performed. As shown in FIG. 5, alpha-Fe of the present invention 2 O 3 Nanowire heteroepitaxy ZnO @ ZIF-8 microporous nano gas-sensitive material pair H 2 S gas exhibits extremely excellent selectivity.
Example 2
Analogously to example 1, with the difference that the ZnO seed layer deposited in one atomic layer had a thickness of 30 nm, alpha-Fe was obtained 2 O 3 SEM characteristic diagram of nano-wire heteroepitaxy ZnO @ ZIF-8 microporous nano material is shown in figure 6, wherein alpha-Fe 2 O 3 The average diameter of the heteroepitaxial ZnO @ ZIF-8 microporous nanowire is about 350 nm, and the average length is more than 10 mu m, so that the finally synthesized alpha-Fe is obtained when the thickness of the ZnO seed crystal layer is increased compared with that of the ZnO seed crystal layer in example 1 2 O 3 The average diameter of the microporous nano of the nanowire hetero-epitaxial ZnO @ ZIF-8 is correspondingly increased, and the microporous nano material ZIF-8 is still uniformly coated on the alpha-Fe 2 O 3 @ ZnO nanowire surface. alpha-Fe obtained by adjusting the thickness of the ZnO seed crystal layer to 30 nm 2 O 3 H is carried out on the nanowire heteroepitaxy ZnO @ ZIF-8 microporous nanomaterial 2 S gas sensing performance test results are shown in FIG. 7, and the response is shown in comparison with the alpha-Fe obtained in example 1 in which the ZnO seed layer has a thickness of 25 nm 2 O 3 The nano-wire heteroepitaxy ZnO @ ZIF-8 microporous nano material is slightly lower, but is relatively pure alpha-Fe 2 O 3 Nanowire and alpha-Fe 2 O 3 The lifting of the @ ZnO core-shell nanowire is still obvious.
The embodiments of the present invention have been described in detail in the above examples, but the present invention is not limited to the specific details in the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
Claims (10)
1. Based on alpha-Fe 2 O 3 The preparation process of the nanowire heteroepitaxy ZnO @ ZIF-8 microporous nanomaterial is characterized by comprising the following specific steps of:
(1) the foamed iron which is cleaned by ultrasonic and dried fully is used as a substrate and a source material, and is put into a muffle furnace for thermal oxidation to obtain alpha-Fe 2 O 3 A nanowire;
(2) the alpha-Fe growing in the step (1) 2 O 3 Placing the foamed iron substrate of the nanowire into an atomic layer deposition system to deposit a ZnO film and provide a seed crystal layer for the subsequent growth of ZIF-8;
(3) reversing the sample prepared by atomic layer deposition in the step (2) into a hydrothermal kettle, epitaxially growing a ZIF-8 nano structure by a solvothermal method, washing with absolute ethyl alcohol after the reaction is finished, and drying to obtain alpha-Fe 2 O 3 The nanowire hetero-epitaxy ZnO @ ZIF-8 microporous nanomaterial is disclosed.
2. The preparation process according to claim 1, wherein in the step (1), the ultrasonic cleaning specifically comprises sequentially performing ultrasonic cleaning with absolute ethyl alcohol and deionized water for 10-15 min; the muffle furnace thermal oxidation process is carried out in the air atmosphere at the growth temperature of 600-800 ℃ for 6-12 hours.
3. The process of claim 1, wherein in step (1), α -Fe is obtained 2 O 3 The average diameter of the nanowires is 60-110 nm, and the average length of the nanowires is 10-15 mu m.
4. The preparation process according to claim 1, wherein in the step (2), the specific process of atomic layer deposition comprises: diethyl zinc DEZ is selected as a zinc source, deionized water is selected as an oxygen source, the reaction temperature is set to be 150-220 ℃, and the growth rate of the ZnO film is set to be 0.20-0.30 nm/cycle finally.
5. The preparation process according to claim 1, wherein in the step (2), the thickness of the atomic layer deposition ZnO film is 5-50 nm.
6. The process according to claim 1, wherein in step (3), the solvent for solvothermal growth is DMF/H in a volume ratio of 3:1 2 And the precursor of the O solution is 2-methylimidazole, the concentration of the precursor solution is 0.05-0.4 mol/L, the growth temperature is 60-80 ℃, and the growth time is 5-10 hours.
7. alpha-Fe-based alloy prepared by the preparation process of claim 1 2 O 3 The nanowire hetero-epitaxy ZnO @ ZIF-8 microporous nanomaterial is disclosed.
8. The microporous nanomaterial of claim 7, wherein the microporous nanowires have an average diameter of 70-400 nm, an average length of 10-15 μm, and an average pore size of 0.3-0.4 nm.
9. Use of the microporous nanomaterial of claim 7 in hydrogen sulfide gas sensing.
10. The use of claim 9, wherein the concentration of detectable hydrogen sulfide gas is between 0.05 and 50 ppm.
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| LI-YUAN ZHU ET AL., 《SMALL》HETEROSTRUCTURED Α-FE2O3@ZNO@ZIF-8 CORE–SHELL NANOWIRES FOR A HIGHLY SELECTIVE MEMS-BASED PPB-LEVEL H2S GAS SENSOR SYSTEM, vol. 18, pages 1 - 14 * |
| 陈萍 等, 《分析化学》微波辅助GO / FE3O4 / ZIF-8磁固相萃取-气相色谱-质谱联用分析薰衣草中的挥发性成分, vol. 50, no. 5, pages 747 - 756 * |
| 陈迎, 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》ZIF-8诱导合成Α-FE2O3基微纳米异质结构及其气敏性质研究, no. 2 * |
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