CN112811472B - Calcium ferrite gas sensing material, preparation method and application - Google Patents
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Abstract
The invention discloses a calcium ferrite gas sensing material, a preparation method and application thereof. The preparation method comprises adding calcium chloride and ferric chloride into mixed solution of ethanol and distilled water at a molar ratio of 1: 2, and magnetically stirring for at least 20 min; transferring the mixture into a reaction kettle, heating the mixture to 140 to 180 ℃, and keeping the temperature for more than 12 hours; after the reaction is finished, cooling to room temperature, and carrying out solid-liquid separation, drying and grinding. The calcium ferrite gas sensing material is synthesized by a simple one-step hydrothermal method, has a unique morphology structure, is in a nanocube structure, is used for detecting reductive gases (formaldehyde, toluene, hydrogen, carbon monoxide, sulfur dioxide, ammonia gas and acetone), shows the most excellent gas-sensitive performance to formaldehyde, and is applied to the technical field of gas detection.
Description
Technical Field
The invention belongs to the technical field of gas detection, and particularly relates to a formaldehyde sensing material and a preparation method of the material.
Background
Formaldehyde is a carcinogenic and teratogenic gas, which can cause serious health problems even at low concentrations. Therefore, the development of a gas sensing material for effectively detecting the concentration of formaldehyde is very important for human health and indoor environmental protection.
CaFe 2 O 4 The (calcium ferrite) is a p-type ternary metal oxide semiconductor material and has the characteristics of excellent conductivity, electron mobility, optical performance, narrow forbidden band width and the like. CaFe 2 O 4 Has shown excellent application in the fields of photocatalysis, electrochemistry, photoelectrochemistry and the like.
According to the document "Orthorhombic CaFe 2 O 4 : A promising p-type gas sensor[J]", A. \352utka, M. Kodu, R. P \228rna, R. Saar, I. Juhnevica, R. Jaaniso, V. Kisand, sens. Initiators B chem. 224 (2016) 260-265. (" orthogonal CaFe. RTM. 2 O 4 Is a promising p-type gas sensor, andruss Sutcard, sensors and activators B Chemical, no. 224, pages 260-265, 2016Year) record: \352utkaet al synthesized CaFe by sol auto-combustion method 2 O 4 Powder of CaFe 2 O 4 A high response (41.5) was shown to 100 ppm ethanol at 200 ℃.
Document "Visible Light-drive p-Type Semiconductor Gas Sensors Based on CaFe 2 O 4 Nanoparticles[J]", qomaruddin, o. Casals, a. \352utka, t. Granz, a. Waag, h.s. Wassto, j.d. Prades, c.f. brega, sensors 20 (2020). (" based on CaFe) 2 O 4 Nanoparticle visible light driven p-type semiconductor gas sensor ", geomarudine, sensors, 20 th, 2020), records: qomaruddin et al synthesized CaFe with nanoparticle structure by sol-gel automatic combustion method 2 O 4 The CaFe 2 O 4 The nano particles keep anisotropic shape, and have uneven particle size and wide distribution range.
Despite CaFe 2 O 4 The gas-sensitive characteristics of the material have been studied in the field of gas sensors, however, caFe with different morphological structures 2 O 4 The gas-sensitive characteristic research for detecting various reducing gases is far from enough.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a calcium ferrite gas sensing material which can effectively detect the concentration of formaldehyde. The invention also provides a preparation method and application of the calcium ferrite gas sensing material.
In order to solve the technical problems, the invention adopts the following technical scheme:
the calcium ferrite gas sensing material provided by the invention is of a nanocube structure.
The invention provides a method for preparing a calcium ferrite gas sensing material, which comprises the following steps:
and 4, carrying out solid-liquid separation, drying and grinding on the product obtained in the step 3 to obtain the nano cubic structure calcium ferrite powder.
The invention also provides the calcium ferrite gas sensing material for detecting the concentration of formaldehyde.
Compared with the existing CaFe 2 O 4 Compared with the materials, the invention has the advantages that:
successful preparation of CaFe by a simple one-step hydrothermal method 2 O 4 A material; the CaFe 2 O 4 Presents a unique nanocube structure; the gas sensitive material is used for detecting reducing gases (formaldehyde, toluene, hydrogen, carbon monoxide, sulfur dioxide, ammonia gas and acetone), and has the most excellent gas sensitive performance on formaldehyde.
Drawings
The drawings of the invention are illustrated as follows:
FIG. 1 shows CaFe 2 O 4 An XRD pattern of (a);
FIG. 2 shows CaFe 2 O 4 XPS spectra of (a);
(a) Is CaFe 2 O 4 XPS full spectrum of (a); (b) Is CaFe 2 O 4 XPS Ca 2p spectrum of (a);
(c) Is CaFe 2 O 4 XPS Fe 2p spectra of (a); (d) Is CaFe 2 O 4 XPS O1 s spectra of (a);
FIG. 3 shows CaFe 2 O 4 N of (2) 2 Adsorption-desorption isotherms;
FIG. 4 shows CaFe 2 O 4 SEM and TEM images of (a);
(a-c) is CaFe 2 O 4 An SEM image of the nanocubes,
(d-f) is CaFe 2 O 4 TEM images of nanocubes;
FIG. 5 shows CaFe 2 O 4 Fabrication flow for base gas sensorA program diagram and a test system diagram;
FIG. 6 shows CaFe 2 O 4 The optimal working temperature of the base gas sensor for 30ppm formaldehyde at different working temperatures (100-400 ℃);
FIG. 7 shows CaFe 2 O 4 Sensitivity of the base gas sensor to 30ppm of different target gases (toluene, hydrogen, formaldehyde, carbon monoxide, sulfur dioxide, ammonia and acetone) at an optimal working temperature;
FIG. 8 shows CaFe 2 O 4 A dynamic response recovery curve of the base gas sensor to formaldehyde gas of 1 to 40 ppm at the optimal temperature;
FIG. 9 (a) shows CaFe 2 O 4 5 cycle response-recovery curves for a base gas sensor at 300 ℃ to 30ppm formaldehyde; (b) Is CaFe 2 O 4 Sensitivity of the gas sensor to 30ppm formaldehyde within 30 days at 300 ℃;
FIG. 10 shows CaFe 2 O 4 Sensitivity of the base gas sensor to 30ppm formaldehyde at 300 ℃ and different humidities:
（a）30% RH，（b）50% RH，（c）70% RH；
FIG. 11 shows CaFe 2 O 4 Ultraviolet-visible absorption spectrum of the sample;
FIG. 12 shows CaFe 2 O 4 Photoluminescence spectra of the sample;
FIG. 13 shows CaFe 2 O 4 Infrared spectroscopy of the sample.
Detailed Description
The invention is further illustrated by the following examples in conjunction with the accompanying drawings:
example 1 (calcium chloride: ferric chloride = 1: 1)
Adding 1 mmol calcium chloride and 1 mmol ferric chloride into a mixed solution of ionized water (10 ml) and ethanol (30 ml), and magnetically stirring for more than 20 minutes; and transferring the uniformly mixed solution into a 50 ml reaction kettle, keeping the temperature at 140 ℃ for 24 hours, naturally cooling the reaction kettle to room temperature after the reaction is finished, and performing solid-liquid separation, drying and grinding to obtain a sample 1.
Example 2 (calcium chloride: ferric chloride = 1: 2)
Adding 1 mmol of calcium chloride and 2 mmol of ferric chloride into a mixed solution of ionized water (10 ml) and ethanol (30 ml), and magnetically stirring for more than 20 minutes; and transferring the uniformly mixed solution into a 50 ml reaction kettle, keeping the temperature at 180 ℃ for 12 hours, naturally cooling the reaction kettle to room temperature after the reaction is finished, and carrying out solid-liquid separation, drying and grinding to obtain a sample 2.
Example 3 (calcium chloride: ferric chloride = 1: 3)
Adding 1 mmol of calcium chloride and 3mmol of ferric chloride into a mixed solution of ionized water (10 ml) and ethanol (30 ml), and magnetically stirring for more than 20 minutes; and transferring the uniformly mixed solution into a 50 ml reaction kettle, keeping the temperature at 160 ℃ for 18 hours, naturally cooling the reaction kettle to room temperature after the reaction is finished, and carrying out solid-liquid separation, drying and grinding to obtain a sample 3.
Sample characterization
By X-ray diffraction (XRD, max-1200, japan), scanning electron microscope (SEM, JEOL model JSM-6490), transmission electron microscope (TEM, JEM-2010), N 2 The crystal phase, the morphology structure, the specific surface area and the chemical composition of the sample were characterized by an adsorption-desorption instrument (ASAP 2020, usa), UV (UV-2700) and X-ray photoelectron spectroscopy (XPS, thermo ESCALAB 250, usa).
Fig. 1 is an XRD pattern of 3 samples, and it can be seen in fig. 1 that the main diffraction peaks 2 θ =24.36 °, 33.24 °, 35.72 °, 40.30 °, 49.60 °, 54.50 °, 57.74 °, 62.52 °, 64.0 ° and 71.9 ° of sample 2 correspond to CaFe, respectively 2 O 4 (220), (320), (201), (131), (401), (260), (600), (170), (261) and (322) crystal planes (JCPDS: 32-0168). In addition, no other impurity peaks were observed, indicating CaFe 2 O 4 High purity of the sample; while the main diffraction peak of sample 1 appeared as beta-FeOOH (JCPDS: 42-1315), not CaFe 2 O 4 A substance; the main diffraction peak of sample 3 is represented by CaFe 2 O 4 、CaFe 5 O 7 、Fe 2 O 3 Is a mixture of impure CaFe 2 O 4 Sample (I). The results show that (example 2) calcium chloride: iron chloride = 1: 2 for optimum molar ratio.
XPS Spectroscopy for characterizing CaFe 2 O 4 The constituent elements and chemical valences of the samples. As shown in FIG. 2 (a), caFe prepared in example 2 2 O 4 The spectrum of sample 2 has Ca, fe, O, and C peaks. FIG. 2 (b) shows CaFe 2 O 4 XPS Ca 2p spectra of (1), two peaks at 348.70 eV and 352.30 eV, respectively, corresponding to Ca 2p 3/2 And Ca 2p 1/2 Indicating that the chemical valence of Ca is +2. FIG. 2 (c) shows CaFe 2 O 4 XPS Fe 2p spectra of (1), with two peaks at 711.30 eV and 725.00 eV, corresponding to Ca 2p 3/2 and Ca 2p 1/2 Indicating that the valence of Fe is +3. FIG. 2 (d) shows CaFe 2 O 4 The XPS O1 s spectra of (A) show two different types of oxygen, namely lattice oxygen and surface adsorbed oxygen, at 530.50 eV and 532.38 eV respectively. The XPS analysis result is consistent with the XRD analysis result, which shows that CaFe is successfully synthesized by a simple one-step hydrothermal method 2 O 4 A material.
FIG. 3 shows CaFe 2 O 4 N of (2) 2 Adsorption-desorption isotherm plot; in FIG. 3, caFe 2 O 4 The material is IV-type isotherm, and the shape of a hysteresis loop on the isotherm is H3 molded line, which indicates that the mesoporous exists in the sample.
FIG. 4 shows CaFe 2 O 4 SEM and TEM of materials. As can be seen in FIG. 4 (a), a large range of CaFe with regular structure and uniform size was successfully synthesized 2 O 4 . In FIG. 4 (b), caFe 2 O 4 Presenting a nanocube structure with an average side length of 470 nm. CaFe 2 O 4 The nanocubes are loosely stacked together and have dispersed particle sizes, so that a plurality of convenient paths can be generated, and the adsorption and desorption of target gas are facilitated. CaFe can be seen in FIG. 4 (c) 2 O 4 The nanocubes have rough surfaces and are distributed with pores. This unique nanocube structure and surface features will expose more active reaction sites, resulting in high sensitivity. In figure 4 (d-f),CaFe can be seen 2 O 4 The edge of the nanocube is clearly black and white, which shows that CaFe 2 O 4 The edges of the sample have a porous structure, this in combination with N 2 The adsorption-desorption isotherms and the results of SEM analysis were consistent.
FIG. 5 shows CaFe 2 O 4 A preparation flow chart and a test system chart of the base gas sensor. FIG. 5 (a) shows CaFe 2 O 4 Preparation flow chart of gas sensor, and CaFe is prepared by adopting brush coating method 2 O 4 A base gas sensor: firstly, a certain amount of CaFe 2 O 4 The sample is added into deionized water to form uniform slurry, the slurry is uniformly coated on the surface of an Ag-Pd fork electrode on an alumina substrate, then the prepared gas sensor is placed on an aging table at 300 ℃ for aging for 1 h, and the gas-sensitive performance of the material is tested after the aging is finished.
FIG. 5 (b) is a test system diagram for testing CaFe by CGS-1TP intelligent gas-sensitive analysis system (Beijing Elite, china) 2 O 4 Based on the performance of the gas sensor, the system consists of a cooling circulation system, a test system, a temperature control system and a data acquisition system, and firstly, a gas sensitive element is placed in the center of a temperature control platform, the position of a probe is adjusted, and the working temperature is set. When the gas sensor resistance is stable, the resistance of the gas sensor in the air is collected
Then injecting the target gas into the test chamber, and obtaining the resistance of the gas sensor in the target gas when the resistance of the gas sensor is stable
Thereby defining the sensitivity of the sample
. Response and recovery times were defined as the time required for the response change to reach 90% of the steady value after test gas entry and removal.
CaFe was tested as shown in FIG. 6 2 O 4 Gas-based sensors operating at different temperatures (1)Sensitivity to 30ppm formaldehyde at 00 ℃ to 400 ℃): caFe 2 O 4 The sensitivity of the base gas sensor increases with the increase of the operating temperature (100 to 300 ℃), reaches the maximum response value (16.50) at 300 ℃, and then gradually decreases when the temperature exceeds 300 ℃. Thus, caFe 2 O 4 The optimum operating temperature and maximum sensitivity value of the base gas sensor were 300 ℃ and 16.50, respectively.
FIG. 7 shows CaFe 2 O 4 Sensitivity of the base gas sensor to 30ppm of different target gases at the optimum operating temperature. As can be seen from FIG. 7, caFe 2 O 4 The base gas sensor has the highest sensitivity to formaldehyde (16.50) to C 7 H 8 （1.44），H 2 （1.30），CO （1.53），SO 2 （1.79），NH 3 (2.15) and C 3 H 6 The sensitivity of O (4.24) is very low (both do not exceed 5), indicating that CaFe 2 O 4 The base gas sensor has good selectivity to formaldehyde.
FIG. 8 shows CaFe 2 O 4 The dynamic response recovery curve of the base gas sensor to formaldehyde gas of 1 to 40 ppm at the optimal temperature is as follows: injecting 1 ppm formaldehyde at 100s, and releasing into the air at 300 s; injecting 5 ppm formaldehyde again at 400s, and releasing into the air at 600 s; at 700s, 10 ppm formaldehyde was again injected, followed in sequence. CaFe 2 O 4 The sensitivity of the base gas sensor to formaldehyde of 1 to 40 ppm corresponded to 3.4 (1 ppm), 5.7 (5 ppm), 8.8 (10 ppm), 10.39 (15 ppm), 11.52 (20 ppm), 14.57 (25 ppm), 16.50 (30 ppm), 18.06 (35 ppm) and 20.75 (40 ppm), respectively. Obviously, caFe 2 O 4 The sensitivity of the base gas sensor increases with increasing HCHO concentration.
FIG. 9 (a) shows CaFe 2 O 4 The base gas sensor has a 5 cycle response-recovery curve at 300 ℃ for 30ppm formaldehyde, test mode: introducing formaldehyde gas for 5 times, and then exchanging air for 5 times. As can be seen from fig. 9 (a): after 5 continuous periods, the sensitivity still maintains the initial response-recovery amplitude, which indicates that CaFe 2 O 4 The base gas sensor has good repeatability for HCHO. FIG. 9 (b) shows CaFe 2 O 4 The sensitivity of the base gas sensor to 30ppm formaldehyde at 300 ℃ over 30 days can be seen: after 30 days, caFe 2 O 4 The sensitivity error of the gas sensor is less than 5 percent, which shows that the CaFe 2 O 4 High stability of the gas-based sensor.
FIG. 10 shows CaFe 2 O 4 Sensitivity of the base gas sensor to 30ppm formaldehyde at 300 ℃ and different humidities: (a) 30% RH, (b) 50% RH, (c) 70% RH, test procedure: formaldehyde gas was injected at 100s, released into the air at 300s, and collection ended at 400 s. In FIGS. 10 (a-c), caFe 2 O 4 The sensitivity and response recovery time of the base gas sensor to 30ppm HCHO were: 16.50 and 153 s-54 s (30% RH), 15.59 and 159 s-64 s (50% RH), 13.76 and 171 s-69 s (70% RH). It can be seen that CaFe 2 O 4 The sensitivity and response recovery time of the gas sensor are slightly changed, and the fact that CaFe 2 O 4 Has excellent moisture resistance.
FIG. 11 shows CaFe 2 O 4 Uv-vis absorption curve of the sample. As shown in FIG. 11, caFe can be obtained by the line-cutting method 2 O 4 Maximum absorption wavelength (722 nm) of the sample, from which the band width can be estimated (
) This indicates that the material is optically active.
FIG. 12 shows CaFe 2 O 4 The photoluminescence spectrum of the sample (the photoluminescence spectrum is mainly used for explaining the recombination rate degree of electrons and holes), it can be seen that the fluorescence mainly appears at 400 to 450 nm, the fluorescence intensity is lower, and the result shows that CaFe 2 O 4 The electron-hole recombination rate of the sample is low, namely the separation efficiency of the current carrier is high.
FIG. 13 shows CaFe 2 O 4 The infrared spectrum of the sample is 3600-3300 cm -1 And 1650 to 1590 cm -1 Peak at (b) indicating-OH groupPresence and absorption of H 2 An O molecule; is positioned at 590-540 cm -1 And 500 to 460cm -1 The peak of (A) is CaFe 2 O 4 Characteristic peaks of Fe-O and Ca-O oscillations of (1); is located at 2347 cm -1 The antisymmetric stretching mode of (b) indicates the presence of dissolved carbon dioxide.
The combination of gas-sensitive properties can result in: caFe of the invention 2 O 4 The material has good gas-sensitive performance, firstly, the CaFe of the invention 2 O 4 The material has unique nanocube structure and surface characteristics, exposes more active reaction sites, and improves the content of CaFe 2 O 4 The sensitivity of (2); caFe 2 O 4 The nanocubes are loosely stacked and dispersed in particle size, providing a plurality of channels for gas diffusion and adsorption/desorption, increasing CaFe 2 O 4 Response recovery characteristics of (a); second, because of CaFe 2 O 4 The narrow forbidden band width and the low electron-hole recombination rate are beneficial to the transition and migration of electrons, so that more oxygen vacancies are possessed, and the gas-sensitive performance of the material is improved.
In conclusion, the simple one-step hydrothermal method is adopted to successfully prepare the CaFe with the nano cubic structure 2 O 4 The gas sensing material is applied to a gas sensor to detect formaldehyde gas, and the result shows that: at an optimum temperature of 300 ℃, caFe 2 O 4 The nanocube material has higher sensitivity (16.50) to 30ppm formaldehyde and quick response recovery time (153 s-54 s), and is a candidate material of a formaldehyde gas sensor.
Claims (2)
1. A preparation method of a calcium ferrite gas sensing material is characterized by comprising the following steps:
step 1, adding calcium chloride and ferric chloride into a mixed solution of ethanol and distilled water according to the molar ratio of 1: 2, and magnetically stirring for at least 20 minutes until the calcium chloride and the ferric chloride are completely dissolved into the solution;
step 2, transferring the uniformly mixed solution obtained in the step 1 into a reaction kettle, heating the solution at the temperature of 140-180 ℃, and keeping the temperature for more than 12 hours;
step 3, after the reaction is finished, cooling the reaction kettle to room temperature;
and 4, carrying out solid-liquid separation, drying and grinding on the product obtained in the step 3 to obtain the nano cubic structure calcium ferrite powder.
2. A calcium ferrite gas sensing material obtained by the production method according to claim 1, which is used for detecting the concentration of formaldehyde.
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