CN111874954A - Gas-sensitive nano material based on carbon particle modified mesoporous iron oxide nanorod structure, preparation process and application thereof - Google Patents
Gas-sensitive nano material based on carbon particle modified mesoporous iron oxide nanorod structure, preparation process and application thereof Download PDFInfo
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Abstract
The invention discloses a gas-sensitive nano material with a mesoporous iron oxide nanorod structure based on carbon particle modification, and a preparation process and application thereof. The invention adopts a self-sacrifice template method to carry out a one-step calcination process on a template material Fe-MOF nanorod prepared by a solvothermal method, so as to obtain a carbon particle modified mesoporous iron oxide nanorod heterostructure. The material preparation method has the advantages of low cost, simple synthesis process, high preparation efficiency, large-scale production and the like. The prepared heterogeneous gas-sensitive nano material can realize ultrasensitive and high-selectivity detection on ppb level trace acetone gas, can be widely applied to monitoring of gas leakage and emission in chemical industry, laboratories and the like, can realize screening of type I diabetes by being applied to human exhaled breath detection, and is applied to the fields of environmental detection and medical health.
Description
Technical Field
The invention relates to the technical field of semiconductor nano material preparation and gas sensing application, in particular to a gas-sensitive nano material based on a carbon particle modified mesoporous iron oxide nanorod structure, a preparation process and application thereof.
Background
In recent years, gas sensing technology plays an important role in various fields such as toxic gas detection, environment monitoring, smoke alarm, automobile exhaust emission control, smart home and the like. With the rapid development of nano science and nano technology, the design of a porous heterogeneous metal oxide nano material with high specific surface area and high porosity as a gas sensitive material has become a hot point of research in the field of gas sensing. Meanwhile, the chemical resistance type gas sensor based on the semiconductor metal oxide nano material has the advantages of low cost, good stability, simple manufacturing process, large-scale preparation and the like, and is attracted by extensive research.
The traditional preparation of porous metal oxide mostly adopts a hard template method. However, the preparation process of the hard template method usually requires the use of expensive and toxic reagents, and the preparation steps are complicated, so that improvement is needed. Therefore, a simple, efficient and morphology-controllable preparation process of porous metal oxide with Metal Organic Framework (MOF) material as a self-sacrificial template has attracted great research interest. The MOF is a porous material and is formed by self-assembling metal ions and organic ligands, has the characteristics of high porosity, large specific surface area and the like, and is beneficial to increasing the adsorption area of gas and improving the sensitivity of a sensing device when being applied to the field of gas sensing. In addition, the composition and morphology of MOF materials can be manipulated by replacing or modifying metal ions and organic ligands. By taking MOF as a self-sacrifice template and carrying out accurately controlled pyrolysis reaction, the porous pure metal oxide MOF derivative material with similar appearance and better retained porosity can be obtained. To the best of our knowledge, no heterogeneous Fe-MOF derived nano material with controllable morphology and composition, namely the carbon particle modified mesoporous iron oxide, is designed and prepared and is used in the field of gas sensing.
Acetone is a volatile organic compound which is used as a polar solvent and is a reaction reagent commonly used in chemical production and laboratories. However, excessive inhalation of acetone gas can inhibit the central nervous system of a human body and cause damage to the health of the human body, so that the realization of trace sensing of acetone has important significance in the field of environmental monitoring. In addition, with the continuous improvement of medical technology, relevant literature reports prove that the accurate detection of the concentration of acetone in exhaled breath of human bodies can screen diseases such as diabetes and the like. Therefore, low cost, high efficiency, high sensitivity and selectivity acetone gas sensors will also play a huge role in noninvasive medical diagnostics in the future.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a gas-sensitive nanomaterial based on a carbon particle-modified mesoporous iron oxide nanorod structure, a preparation process and application thereof. The invention provides a novel, simple and efficient synthesis route for large-scale preparation of a carbon particle modified mesoporous iron oxide nanorod heterogeneous nanomaterial. The method adopts an advanced self-sacrifice template idea and a simple and efficient one-step calcination pyrolysis technology, has the advantages of low cost, high preparation efficiency, high repeatability and the like, and provides a brand new idea for preparing the porous heterogeneous gas-sensitive nano material in a large scale. The carbon particle modified mesoporous iron oxide nanorod material prepared by the invention has the characteristics of high porosity, large specific surface area, sensitive response, good selectivity and good stability as a gas sensitive material.
In the invention, the preparation of the self-sacrifice template material Fe-MOF nanorod adopts a solvothermal method, and a final product, namely the carbon particle modified mesoporous iron oxide nanorod is obtained through a one-step calcination process with simple and easily-controlled synthesis conditions. The technical solution of the present invention is as follows.
The invention provides a preparation process of a carbon particle modified mesoporous iron oxide nanorod structure gas-sensitive nanomaterial, which comprises the following specific steps:
(1) preparing a mixed aqueous solution A with the concentration of F127 being 0.009-0.012 g/mL and the concentration of ferric trichloride hexahydrate being 0.010-0.015 g/mL;
(2) stirring the mixed solution A prepared in the step (1) for 0.5-2 hours, and then injecting a proper amount of anhydrous acetic acid to obtain a mixed solution B;
(3) stirring the mixed solution B prepared in the step (2) for 0.5-2 hours, and adding a proper amount of 2-amino terephthalic acid solid to obtain a mixed solution C;
(4) stirring the mixed solution C prepared in the step (3) for 1-3 hours, taking the mixed solution C as a precursor solution, pouring the mixed solution C into a hydrothermal kettle for solvothermal reaction, cleaning the solution with ethanol for a plurality of times after the solvothermal reaction is finished, and drying the solution to obtain a self-sacrifice template material Fe-MOF nanorod;
(5) completely drying the Fe-MOF nano rod obtained in the step (4) at room temperature or in an oven, and then putting the sample into a muffle furnace for calcining; after calcining and sintering, naturally cooling to room temperature to obtain the carbon particle modified mesoporous iron oxide nanorod heterogeneous gas-sensitive nano material.
In the step (2), the volume ratio of the anhydrous acetic acid to the mixed solution A is 0.03-0.05.
In the step (3), the concentration of the 2-amino terephthalic acid is 0.003 to 0.005 g/mL.
In the step (4), the growth temperature of the solvothermal reaction is 100-120 ℃, and the growth time is 12-36 hours.
In the step (4), the average diameter of the obtained Fe-MOF nano rod is 70-100 nm, and the average length is 500-600 nm.
In the step (5), when the drying oven is adopted for drying, the setting temperature of the drying oven is not higher than 80 ℃.
In the step (5), the calcining temperature of the muffle furnace is 250-350 ℃, and the calcining time is 1-3 h.
The invention also provides a gas-sensitive nano material based on the carbon particle modified mesoporous iron oxide nanorod structure, which is prepared by the preparation process. The average diameter of the carbon particle modified mesoporous iron oxide nanorod is 50-80 nm, the average length of the carbon particle modified mesoporous iron oxide nanorod is 450-550 nm, the average diameter of mesopores is 3-5 nm, and the average diameter of carbon particles is 5-10 nm.
The invention further provides an application of the gas-sensitive nano material based on the carbon particle modified mesoporous iron oxide nanorod structure in the aspect of detecting acetone gas.
Compared with the prior art, the invention has the beneficial effects that:
1. compared with a pure MOF material, the derivative is obtained by taking the MOF material as a self-sacrifice template through a one-step calcination method, the chemical stability and the thermal stability of the derivative are greatly improved, the contradiction that the pure MOF material has poor room temperature response and poor thermal stability at higher working temperature is overcome, and the long-term stability and the service life of a gas sensing device are favorably improved.
2. Compared with other single metal oxide MOF derivative materials, the carbon particle modified mesoporous iron oxide nanorod material forms a carbon @ oxide heterostructure on the basis of effectively increasing the porosity and the specific surface area of the material, so that the gas-sensitive response of the material can be further improved; meanwhile, the conductivity of carbon is far better than that of a metal oxide semiconductor material, and the response/recovery speed of the material to the detection gas can be effectively improved by carbon particle modification.
3. The preparation process of the novel porous heterogeneous material combines the solvothermal method with a one-step calcining method with simple and efficient synthesis process, creatively utilizes the idea of self-sacrifice template, not only effectively overcomes the problems of high complexity and high cost of the traditional hard template preparation process, but also has the advantages of good repeatability, high preparation efficiency, suitability for large-scale preparation and the like.
4. The heterogeneous gas-sensitive nanomaterial of the carbon particle-modified mesoporous iron oxide nanorod structure can realize ultrasensitive and high-selectivity detection on 0.5-2.5 ppm trace acetone, and on one hand, the heterogeneous gas-sensitive nanomaterial plays an important role in the field of environmental monitoring; on the other hand, the detectable range of the acetone gas completely covers different distribution of the acetone concentration in the exhaled breath of healthy human bodies and type I diabetic patients, so that the acetone gas plays a great role in noninvasive medical diagnosis in the future.
Drawings
FIG. 1 is a flow chart of a preparation process of a heterogeneous gas-sensitive nanomaterial based on a carbon particle-modified mesoporous iron oxide nanorod structure.
FIG. 2 is an SEM representation of Fe-MOF nanorods obtained in example 1.
FIG. 3 is an SEM representation of the carbon particle-modified mesoporous iron oxide nanorods obtained in example 1.
FIG. 4 is a TEM representation of the carbon particle-modified mesoporous iron oxide nanorods obtained in example 1.
FIG. 5 is a trace acetone gas-sensitive performance test result of the two devices of the simple Fe-MOF nanorods and the mesoporous iron oxide nanorods modified by carbon particles obtained in example 1.
Fig. 6 is a graph showing the results of the selective gas-sensitive test of the carbon particle-modified mesoporous iron oxide nanorod gas sensing device obtained in example 1 on seven common harmful gases (acetone, nitrogen dioxide, hydrogen sulfide, ammonia, toluene, methane, and formaldehyde).
FIG. 7 is an SEM representation of the carbon particle-modified mesoporous iron oxide nanorods obtained in example 2.
Fig. 8 is a trace acetone gas-sensitive performance test result diagram of the carbon particle-modified mesoporous iron oxide nanorod gas sensing device obtained in example 2.
Detailed Description
The invention is described in further detail below with reference to the figures and examples.
The flow block diagram of the preparation process of the heterogeneous gas-sensitive nanomaterial based on the carbon particle-modified mesoporous iron oxide nanorod structure is shown in fig. 1.
Example 1
(1) Adding 0.32 g F127 g and 0.358 g ferric chloride hexahydrate into 30 mL deionized water, and uniformly mixing to obtain a mixed solution A;
(2) stirring the mixed solution A prepared in the step (1) for 1 hour, and then injecting 1.2mL of anhydrous acetic acid to obtain a mixed solution B;
(3) stirring the mixed solution B prepared in the step (2) for 1 hour, and then adding 0.12g of 2-amino terephthalic acid solid to obtain a mixed solution C;
(4) stirring the mixed solution C prepared in the step (3) for 2 hours, pouring the mixed solution C as a precursor solution into a hydrothermal kettle, carrying out solvothermal reaction for 24 hours at 110 ℃, cleaning for several times by using ethanol after the solvothermal reaction is finished, and drying by blowing to obtain the Fe-MOF nanorod as the self-sacrifice template material, wherein an SEM representation picture is shown in figure 2, and the Fe-MOF nanorod has the average diameter of about 86nm and the average length of about 540 nm;
(5) completely drying the Fe-MOF nano rod of the self-sacrifice template material obtained in the step (4) at room temperature, and then calcining the sample in a muffle furnace at 300 ℃ for 2 hours; after calcination, the carbon particles are naturally cooled to room temperature, and the mesoporous iron oxide nanorods modified by the carbon particles are obtained, wherein SEM images and TEM images of the mesoporous iron oxide nanorods are shown in FIGS. 3 and 4, so that the carbon particles are uniformly modified on the surfaces of the mesoporous iron oxide nanorods, the average diameter of the mesoporous iron oxide nanorods is about 62 nm, the average length of the mesoporous iron oxide nanorods is about 501nm, the average pore diameter of the mesopores is about 3 nm, and the average diameter of the carbon particles is about 6 nm.
In the embodiment, the obtained pure Fe-MOF nanorods and the mesoporous iron oxide nanorods modified by carbon particles are respectively used for carrying out gas sensing test on 0.5-2.5 ppm of acetone gas.
As shown in fig. 5, the test results are as follows: the response value (defined as R) of the mesoporous iron oxide nanorods modified by the carbon particles to 2.5ppm of acetone gasa/RgWherein R isaIs resistance in air, RgResistance in gas to be detected) is 5.2, and the response value of a pure Fe-MOF nanorod is 2.5, the result shows that the sensing response of the carbon particle modified mesoporous iron oxide nanorod heterogeneous gas-sensitive material to 2.5ppm acetone gas is improved by more than 2 times, and the sensitivity of the material to acetone gas at other concentrations is improved to different degrees. Meanwhile, test results show that the detection limit of the carbon particle modified mesoporous iron oxide nanorod heterogeneous gas-sensitive material on acetone gas is at least as low as ppb magnitude, and trace detection on acetone gas can be realized.
In addition, the obtained carbon particle modified mesoporous iron oxide nanorod heterogeneous gas sensitive material is subjected to selectivity test, namely, the gas sensing test is respectively carried out on acetone, nitrogen dioxide, hydrogen sulfide, ammonia gas, toluene, methane and formaldehyde with the same concentration (2.5 ppm). As shown in fig. 6, the carbon particle modified mesoporous iron oxide nanorod heterogeneous gas-sensitive material of the present invention exhibits extremely excellent selectivity for acetone gas.
Example 2
Similar to example 1, except that the calcination temperature in one-step calcination was 350 ℃. The SEM characterization graph of the obtained mesoporous iron oxide nanorods modified by carbon particles is shown in fig. 7, wherein the average diameter of the mesoporous iron oxide nanorods is about 52 nm, the average length is about 436nm, the average pore diameter of the mesopores is about 5nm, and the average diameter of the carbon particles is about 5nm, and it is known that when the calcination temperature is increased compared to example 1, the average diameter and the average length of the mesoporous iron oxide nanorods modified by carbon particles obtained by calcination should be shortened, the size of the mesopores is increased, the average size of the carbon particles is decreased, and the surface distribution concentration is decreased. Acetone gas sensing performance tests are also carried out on the mesoporous iron oxide nanorods modified by the carbon particles obtained by calcination at 350 ℃, and the results are shown in fig. 8, and although the responses of the mesoporous iron oxide nanorods are slightly lower than those of the mesoporous iron oxide nanorods modified by the carbon particles obtained by calcination at 300 ℃ in example 1, the responses are obviously improved compared with those of the simple Fe-MOF nanorods.
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. A preparation process of a gas-sensitive nano material based on a carbon particle modified mesoporous iron oxide nanorod structure is characterized by comprising the following specific steps of:
(1) preparing a mixed aqueous solution A with the concentration of F127 being 0.009-0.012 g/mL and the concentration of ferric trichloride hexahydrate being 0.010-0.015 g/mL;
(2) stirring the mixed solution A prepared in the step (1) for 0.5-2 hours, and then injecting a proper amount of anhydrous acetic acid to obtain a mixed solution B;
(3) stirring the mixed solution B prepared in the step (2) for 0.5-2 hours, and adding a proper amount of 2-amino terephthalic acid solid to obtain a mixed solution C;
(4) stirring the mixed solution C prepared in the step (3) for 1-3 hours, taking the mixed solution C as a precursor solution, pouring the mixed solution C into a hydrothermal kettle for solvothermal reaction, cleaning the solution with ethanol for a plurality of times after the solvothermal reaction is finished, and drying the solution to obtain a self-sacrifice template material Fe-MOF nanorod;
(5) completely drying the Fe-MOF nano rod obtained in the step (4) at room temperature or in an oven, and then putting the sample into a muffle furnace for calcining; after calcining and sintering, naturally cooling to room temperature to obtain the carbon particle modified mesoporous iron oxide nanorod heterogeneous gas-sensitive nano material.
2. The process according to claim 1, wherein in the step (2), the volume ratio of the anhydrous acetic acid to the mixed solution A is 0.03:1 to 0.05:.
3. The process according to claim 1, wherein the concentration of the 2-aminoterephthalic acid added in the step (3) is 0.003 to 0.005 g/mL.
4. The preparation process according to claim 1, wherein in the step (4), the growth temperature of the solvothermal reaction is 100 to 120 ℃ and the growth time is 12 to 36 hours.
5. The preparation process of claim 1, wherein in the step (4), the obtained Fe-MOF nanorods have an average diameter of 70-100 nm and an average length of 500-600 nm.
6. The preparation process according to claim 1, wherein in the step (5), when the oven is used for drying, the setting temperature of the oven is not higher than 80 ℃; the calcining temperature of the muffle furnace is 250-350 ℃, and the calcining time is 1-3 h.
7. The gas-sensitive nanomaterial based on the carbon particle-modified mesoporous iron oxide nanorod structure prepared by the preparation process of claim 1.
8. The gas-sensitive nanomaterial as claimed in claim 7, wherein the mesoporous iron oxide nanorods have an average diameter of 50-80 nm, an average length of 450-550 nm, an average pore diameter of 3-5 nm, and an average diameter of 5-10 nm.
9. Use of the gas-sensitive nanomaterial of claim 7 in acetone gas detection.
10. The use of claim 9, wherein the concentration of detectable acetone gas is between 0.1 and 20 ppm.
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| CN113945611A (en) * | 2021-09-06 | 2022-01-18 | 复旦大学 | Heterogeneous gas-sensitive nano material based on cerium oxide particle modified copper oxide nanowire structure, preparation process and application thereof |
| CN114292410A (en) * | 2021-12-14 | 2022-04-08 | 山东省分析测试中心 | Fe2O3@ Fe-MOF core-shell nanorod and preparation method and application thereof |
| CN115724473A (en) * | 2022-10-09 | 2023-03-03 | 安徽信息工程学院 | Method for preparing ferric oxide nano-rod by MOF room temperature conversion |
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