CN111348677A - Preparation method and application of zinc metastannate nanofiber gas-sensitive material - Google Patents
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Abstract
The invention discloses a preparation method and application of a zinc metastannate nanofiber gas-sensitive material, belongs to the field of preparation of functional ceramic materials, and particularly relates to ZnSnO with a high specific surface area3A preparation method and application of a nanofiber gas-sensitive material. The invention adopts a stirring-hydrothermal method, zinc salt and stannate solution are uniformly mixed according to a certain proportion, the pH value is adjusted, and then the mixture is transferred into a hydrothermal reaction kettle to react under the set time, temperature and stirring speed; after the reaction is finished, filtering, washing and drying to obtain ZnSnO with high specific surface area3And (3) nano fibers. The invention provides a method for synthesizing ZnSnO with high specific surface area3The method for preparing the nano-fiber has the advantages of simple process, convenient operation, high purity and yield and easy industrial large-scale production; and the resulting ZnSnO3The nano-fiber has small diameter and specific surfaceThe product has large volume and loose structure, shows excellent gas-sensitive performance to formaldehyde, can be used in the field of formaldehyde gas sensors, and is suitable for popularization and application.
Description
Technical Field
The invention belongs to the technical field of functional ceramic material preparation, and relates to ZnSnO with a high specific surface area3A preparation method of a nanofiber gas-sensitive material, and simultaneously relates to ZnSnO with high specific surface area3The application of the nanofiber gas-sensitive material in a gas sensor.
Background
With the enhancement of environmental protection and safety awareness, people have recognized that accurate, rapid and real-time detection and early warning of toxic, combustible and explosive gases in the environment are extremely important. Although the detection and early warning of toxic, combustible and explosive gases are widely applied to industrial and mining enterprises, public places and individual families at present, poisoning or damage events caused by toxic and harmful gases and fire or explosion events caused by combustible and explosive gases occur sometimes. The gas sensor is a functional element for detecting and early warning various harmful gases, and although various harmful gas sensors appear in the current market, the current many harmful gas sensitive materials have obvious defects, so that the requirements of real-time detection and early warning of harmful gases cannot be completely met. Therefore, research and development of novel gas sensitive materials have important practical significance for preparing high-performance gas sensors.
ZnSnO3The ternary composite oxide semiconductor material has excellent performance and has important application in the fields of gas sensitivity, catalysis, flame retardance, lithium batteries and the like. ZnSnO3The gas-sensitive mechanism belongs to a surface resistance control model, and is a property closely related to the surface, namely the surface structure and the specific surface area are main factors influencing the gas-sensitive property. Therefore, the nano ZnSnO with high specific surface area is prepared by different synthesis techniques3Is an important measure for improving the gas sensitivity. ZnSnO3The specific surface area of the ZnSnO is related to factors such as the shape structure, the grain size and the like of the material, and in order to obtain high-performance ZnSnO3The research on the synthesis of nano materials by researchers has never been stopped, at present, ZnSnO3The synthesis research of various shapes and structures of nano rods, nano sheets, nano spheres and the like is reported: such as ZnSnO synthesized by Y.J.Chen et al3The specific surface area of the nano-sheet is 57.86m2.g-1(y.j.chen, l.yu, q.li, y.wu, q.h.land t.h.wang, Nanotechnology,2012,23, 415501); ZnSnO reported by X.H.Jiana et al3The specific surface area of the nano hollow sphere is 30.21m2.g-1(x.h.jiaa, m.g.tiana, r.r.dai, d.d.lian, s.han, x.y.wu and h.h.song, sens.actuators, B,2017,240,376); ZnSnO prepared by W.W.Guo et al3The specific surface area of the nano mesoporous hollow cube is 66.9m2.g-1(W.W.Guo,J.Electrochem.Soc.,2016,163,131) (ii) a T.T.ZHou and the like to synthesize nano ZnSnO3The specific surface area of the single-shell cube, the nano double-shell cube and the nano multi-shell cube is 70m2.g-1、86m2.g-1、98m2.g-1(t.t.zhou, t.zhang, r.zhang, z.lou, j.n.deng and l.l.wang, acsappl.mater.interfaces,2017,9, 14525); Y.F.Bing, etc. synthesized mesoporous ZnSnO3Nanocrystal specific surface area of 96m2.g-1(y.f. bing, y.zeng, c.liu, l.qiao, y.m.sui, b.zou, w.t.zheng and g.t.zou, sens.actuators, B,2014,190,370); mesoporous ZnSnO synthesized by Bingshan Wang et al3The specific surface area of the nano-sheet is 105.3m2.g-1(Bingshan Wang, Jinbao Yu, Xiaohong Li, Jun Yinaand Men Chen, RSCAdv.,2019,9,14809-14816) but has a high specific surface area of ZnSnO-3The synthesis of the nano-fiber is not reported in domestic and foreign literatures.
Furthermore, ZnSnO3The synthesis methods mainly comprise the following steps: hydrothermal method, solid-phase high-temperature reaction, magnetron sputtering method, electrostatic spinning method and the like, wherein the hydrothermal method is mainly widely utilized by the advantages of simple synthesis method, easy acquisition of devices, easy control of conditions and the like, and is convenient for industrial production, but the traditional synthesis method is difficult to obtain ZnSnO with high specific surface area3Crystals, some of which are not suitable for scale-up for industrial production.
Therefore, how to provide the nano ZnSnO with high specific surface area, which has simple process, convenient operation and suitability for industrial popularization3The preparation method of (A) is a technical problem to be solved by the technical personnel in the field.
Disclosure of Invention
The invention aims to provide a preparation method of a zinc metastannate nanofiber gas-sensitive material, and ZnSnO with high specific surface area can be successfully obtained by the method3The nano-fiber has simple process and convenient operation, and is suitable for industrial popularization and use.
In order to achieve the technical effects, the invention adopts the following technical scheme:
the invention provides ZnSnO3The preparation method of the nanofiber gas-sensitive material comprises the following steps:
(1) weighing zinc salt and stannate with formula amount, and preparing the zinc salt and the stannate into solutions respectively to obtain a stannate solution and a zinc salt solution for later use;
(2) dropwise adding the stannate solution into the zinc salt solution, stirring, and uniformly mixing to obtain a mixed solution;
(3) the mixed solution is moved into a reaction kettle for hydrothermal reaction after the pH value of the mixed solution is adjusted, and then the mixed solution is cooled, filtered, washed and dried to obtain ZnSnO3A nanofiber gas sensitive material.
In conclusion, the invention adopts a stirring-hydrothermal method, zinc salt and stannate solution are uniformly mixed according to a certain proportion, the pH value is adjusted, and then the mixture is transferred into a hydrothermal reaction kettle to react under the set time, temperature and stirring speed; after the reaction is finished, filtering, washing and drying to obtain ZnSnO with high specific surface area3And (3) nano fibers. Specific ZnSnO3The formation mechanism of (a) is as follows:
SnO3 2-+2H2O→H2SnO3+2OH-
Zn2++4H2O→Zn(OH)4 2-+4H+
H2SnO3+Zn(OH)4 2-+2H+→ZnSn(OH)6↓+H2O
ZnSn(OH)6→ZnSnO3↓+H2O
ZnSnO prepared by the invention3The diameter of the nano-fiber is 2-5 nm, the length-diameter ratio is more than 50, the structure is loose, and the fiber density is less than 0.3g/cm3Specific surface area of more than 190m2·g-1。
Preferably, in the step (1), the zinc salt is zinc acetate, zinc nitrate or zinc chloride; the stannate is sodium stannate or potassium stannate; and the molar ratio of the zinc salt to the stannate is 1: 1, and the concentration of the stannate solution and the concentration of the zinc salt solution are both 0.1-0.2 mol/L.
Wherein, the molar ratio of the zinc salt to the stannate is just 1, and if the ratio of the zinc salt to the stannate is less than 1, SnO can be occluded in the product2Impurities, and if bothIf the ratio is greater than 1, ZnO impurities are generated, and the purity and yield of the product are reduced.
Preferably, in the step (2), in order to avoid the generation of the precipitate during the dropping process or in order to enable the precipitate generated during the dropping process to dissolve and disappear, the dropping rate is less than 3 drops/second, and the stannate solution can only be added into the zinc salt solution dropwise and stirred continuously, otherwise, the precipitate is generated.
Preferably, in the step (3), the pH of the mixed solution before the hydrothermal reaction is 6-8.
Preferably, the hydrothermal reaction temperature is 240-280 ℃, the reaction time is 16-24 h, and the reaction stirring speed is 80-150 r/min.
In addition, the invention also discloses the ZnSnO for protecting the ZnSnO3The application of the nanofiber gas-sensitive material in a gas sensor.
In some application scenarios, the ZnSnO3The nanofiber has excellent gas sensitivity to formaldehyde, the responsivity to 0.2ppm of formaldehyde is over 3 at the optimal working temperature of 220 ℃, the responsivity to 50ppm of formaldehyde is over 50, and the response recovery time is short.
ZnSnO3The wide-bandgap N-type semiconductor is a wide-bandgap N-type semiconductor, and many researches on the gas-sensitive performance of the wide-bandgap N-type semiconductor on formaldehyde are reported in recent years, and the gas-sensitive mechanism belongs to a surface control model. The surface control sensitivity mechanism includes two stages: the first stage is sensitization stage, when the semiconductor element is exposed to air, oxygen is chemisorbed at a certain temperature to extract electrons from the semiconductor conduction band to form O in chemisorption state2-、O-、O2 -Or O2 2-Increasing the resistance of the material; the second stage is a detection stage, in which harmful gases such as formaldehyde and the like react with the adsorbed oxygen ions to ZnSnO3The oxide semiconductor releases electrons, and the resistance of the material decreases. Generally, under the condition that the shape and structure of the same material are the same, the gas-sensitive performance of the material can be judged by comparing the specific surface area, for example, the specific surface area of a large-particle material is small, and the gas-sensitive performance is poor. Therefore, the zinc metastannate nanofiber material prepared by the method disclosed by the invention has very high specific surface areaHas excellent gas-sensitive performance.
According to the technical scheme, compared with the prior art, the preparation method and the application of the zinc metastannate nanofiber gas-sensitive material disclosed by the invention have the following excellent effects:
(1) the method is completely carried out in the aqueous solution, has high purity and yield, does not need any additive or expensive surfactant, and has low cost;
(2) in the preparation process, toxic and harmful substances are not generated in each step, so that the environment is protected, and high-temperature calcination is not needed;
(3) the method is simple, convenient to operate and easy for industrial large-scale production;
(4) the invention adopts a hydrothermal method to synthesize ZnSnO for the first time3The nano-fiber has small length-diameter ratio, large specific surface area and loose structure, shows excellent gas-sensitive performance to formaldehyde and can be used in the field of formaldehyde gas sensors.
Drawings
In order to more clearly illustrate the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, and it is apparent that the drawings in the following description are only embodiments of the present invention, and it is obvious to those skilled in the art that other drawings can be obtained according to the provided drawings without inventive labor.
FIG. 1 is a transmission electron micrograph of a product prepared in example 1 of the present invention.
FIG. 2 is a graph showing the response of gas sensing devices prepared according to example 1 of the present invention to different concentrations of formaldehyde.
FIG. 3 is a transmission electron micrograph of a product prepared in example 2 of the present invention.
FIG. 4 is a transmission electron micrograph of a product prepared in example 3 of the present invention.
Figure 5 is an XRD profile of example products prepared according to the present invention where a is example 1 and b is example 2.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention and the accompanying drawings of the specification, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention discloses a preparation method of a zinc metastannate nanofiber gas-sensitive material, which specifically comprises the following steps:
step 1: respectively weighing a certain amount of zinc salt and stannate to prepare solutions, dropwise adding the stannate solution into the zinc salt solution, continuously stirring, uniformly mixing, and adjusting the pH value to 6-8 for later use;
step 2: transferring the mixed solution into a 100ml stainless steel hydrothermal reaction kettle, sealing, and carrying out hydrothermal reaction at set time, temperature and stirring speed;
and step 3: naturally cooling after the hydrothermal reaction is finished, filtering, repeatedly washing with deionized water, and drying the sample at 75 ℃ to obtain ZnSnO with high specific surface area3And (3) nano fibers.
In order to further optimize the technical scheme, the zinc salt in the step 1 is analytically pure zinc acetate or zinc nitrate or zinc chloride, and the stannate is analytically pure sodium stannate or potassium stannate; and the certain amount of the zinc salt and stannate solution refers to the molar ratio of the zinc salt to the stannate being 1: 1, the concentrations of the zinc salt solution and the zinc stannate solution are both 0.1 mol/L-0.2 mol/L.
Further, the setting time in the step 2 is 16-24 h; setting the temperature to 240-280 ℃; setting the stirring speed to be 80 r/min-150 r/min.
Further, ZnSnO with high specific surface area in step 23The diameter of the nanofiber is 2 nm-5 nm, the length-diameter ratio is more than 50, the structure is loose, and the density is less than 0.3g/cm3Specific surface area of more than 190m2·g-1。
The technical solutions and advantages of the present invention are further illustrated below with reference to specific examples, but the present invention is not limited to the following examples.
Example 1
A preparation method of a zinc metastannate nanofiber gas-sensitive material specifically comprises the following steps:
step 1: weighing 1.65g of zinc acetate dihydrate and 2.14g of sodium stannate tetrahydrate, preparing 50mL of solutions respectively, dropwise adding the sodium stannate solution into the zinc acetate solution, continuously stirring, uniformly mixing, and adjusting the pH value to 6-8 for later use;
step 2: transferring the mixed solution into a 100mL stainless steel hydrothermal reaction kettle, sealing, and reacting for 24h at a set temperature of 240 ℃ and a stirring speed of 100 revolutions per minute;
and step 3: naturally cooling after the hydrothermal reaction is finished, filtering, repeatedly washing with deionized water, and drying the sample at 75 ℃ to obtain ZnSnO with high specific surface area3And (3) nano fibers.
ZnSnO in example 13The diameter of the nano-fiber is 2nm to 5nm, the length-diameter ratio is more than 50, the structure is loose (figure 1), and the density is 0.28g/cm3Specific surface area 198m2·g-1The yield was 96%.
ZnSnO in example 13The nanofiber is applied to a gas sensor, and the gas-sensitive performance of the manufactured gas sensor on formaldehyde is tested. According to the experimental result, under the condition that the optimal working temperature is 220 ℃, the response to 0.2ppm formaldehyde is about 3.1, the response to 50ppm formaldehyde reaches 50.4, the response recovery time is short (figure 2), the material shows excellent gas-sensitive performance to formaldehyde, and the good gas-sensitive characteristic of the material is derived from the large specific surface area, high permeability and the like of the material.
The American national institute of Industrial health (ACGIH) specifies the concentration of toxic and harmful gases in the working environment, wherein formaldehyde is allowed to exist at a maximum average concentration of 0.3ppm and a short contact time limit of 2ppm, and the material can be used for rapidly and effectively detecting formaldehyde gas in the air.
Example 2:
a preparation method of a zinc metastannate nanofiber gas-sensitive material specifically comprises the following steps:
step 1: weighing 1.49g of zinc nitrate hexahydrate and 1.48g of potassium stannate trihydrate, preparing 50mL of solutions respectively, dropwise adding the potassium stannate solution into the zinc nitrate solution, continuously stirring, uniformly mixing, and adjusting the pH value to 6-8 for later use;
step 2: transferring the mixed solution into a 100mL stainless steel hydrothermal reaction kettle, sealing, and reacting for 18h at a set temperature of 250 ℃ and a stirring speed of 100 revolutions per minute;
and step 3: naturally cooling after the hydrothermal reaction is finished, filtering, repeatedly washing with deionized water, and drying the sample at 75 ℃ to obtain ZnSnO with high specific surface area3And (3) nano fibers.
ZnSnO in example 23The diameter of the nano-fiber is 2nm to 5nm, the length-diameter ratio is more than 50, the structure is loose (figure 3), and the density is 0.27g/cm3Specific surface area 201.2m2·g-1The yield was 98%.
ZnSnO in example 23The nanofiber is applied to a gas sensor, and the gas-sensitive performance of the manufactured gas sensor on formaldehyde is tested. According to the experimental result, under the condition that the optimal working temperature is 220 ℃, the responsivity to 0.2ppm formaldehyde is about 3.3, the responsivity to 50ppm formaldehyde reaches 51.7, the response recovery time is short, the material has excellent gas-sensitive performance to formaldehyde, and the good gas-sensitive characteristic of the material is derived from the large specific surface area, high permeability and the like of the material.
Example 3:
a preparation method of a zinc metastannate nanofiber gas-sensitive material specifically comprises the following steps:
step 1: weighing 1.36g of zinc chloride and 2.85g of sodium stannate tetrahydrate, preparing 50mL of solution respectively, dropwise adding the sodium stannate solution into the zinc chloride solution, continuously stirring, uniformly mixing, and adjusting the pH value to 6-8 for later use;
step 2: transferring the mixed solution into a 100mL stainless steel hydrothermal reaction kettle, sealing, and reacting for 16h at a set temperature of 270 ℃ and a stirring speed of 100 revolutions per minute;
and step 3: naturally cooling after the hydrothermal reaction is finished, filtering, repeatedly washing with deionized water, and drying the sample at 75 ℃ to obtain ZnSnO with high specific surface area3And (3) nano fibers.
ZnSnO in example 33The diameter of the nano-fiber is 2nm to 5nm, the length-diameter ratio is more than 50, the structure is loose (figure 4), and the density is 0.28g/cm3Specific surface area of 200.6m2·g-1The yield was 96%.
ZnSnO in example 33The nanofiber is applied to a gas sensor, and the gas-sensitive performance of the manufactured gas sensor on formaldehyde is tested. According to the experimental result, under the condition that the optimal working temperature is 220 ℃, the responsivity to 0.2ppm formaldehyde is about 3.1, the responsivity to 50ppm formaldehyde reaches 52.1, the response recovery time is short, the material has excellent gas-sensitive performance to formaldehyde, and the good gas-sensitive characteristic of the material is derived from high permeability, large specific surface area and the like of the material.
XRD tests are respectively carried out on the products prepared in the examples 1-3, and the results are shown in figure 5 (wherein a is example 1, b is example 2, and the XRD patterns of the example 3 are similar to those of a and b), the XRD patterns of the final products of the three preparation methods and the ZnSnO of a cubic system3The results are completely coincident, and no impurity peak appears, which indicates that the ZnSnO of high-purity cubic system is adopted in the embodiments 1-3 of the invention3。
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The method disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the description of the method part.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (7)
1. ZnSnO3Nano meterThe preparation method of the fiber gas-sensitive material is characterized by comprising the following steps:
(1) weighing zinc salt and stannate with formula amount, and preparing the zinc salt and the stannate into solutions respectively to obtain a stannate solution and a zinc salt solution for later use;
(2) dropwise adding the stannate solution into the zinc salt solution, stirring, and uniformly mixing to obtain a mixed solution;
(3) the mixed solution is moved into a reaction kettle for hydrothermal reaction after the pH value of the mixed solution is adjusted, and then the mixed solution is cooled, filtered, washed and dried to obtain ZnSnO3A nanofiber gas sensitive material.
2. A ZnSnO according to claim 13The preparation method of the nanofiber gas sensitive material is characterized in that in the step (1), the zinc salt is zinc acetate, zinc nitrate or zinc chloride; the stannate is sodium stannate or potassium stannate; and the molar ratio of the zinc salt to the stannate is 1: 1, and the concentration of the stannate solution and the concentration of the zinc salt solution are both 0.1-0.2 mol/L.
3. A ZnSnO according to claim 13The preparation method of the nanofiber gas-sensitive material is characterized in that in the step (2), the dropping speed is less than 3 drops/second.
4. A ZnSnO according to claim 13The preparation method of the nanofiber gas-sensitive material is characterized in that in the step (3), the pH of the mixed solution before hydrothermal reaction is 6-8.
5. ZnSnO according to claim 43The preparation method of the nanofiber gas-sensitive material is characterized in that the hydrothermal reaction temperature is 240-280 ℃, the reaction time is 16-24 hours, and the reaction stirring speed is 80-150 r/min.
6. ZnSnO prepared by the process of claim 13The application of the nanofiber gas-sensitive material in a gas sensor.
7. A ZnSnO according to claim 63Use of a nanofibrous gas-sensitive material, characterized in that the ZnSnO is3The nanofiber has excellent gas sensitivity to formaldehyde, the responsivity to 0.2ppm of formaldehyde is over 3 at the optimal working temperature of 220 ℃, the responsivity to 50ppm of formaldehyde is over 50, and the response recovery time is short.
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| CN113697846A (en) * | 2021-08-05 | 2021-11-26 | 湖北工程学院 | ZnSnO3Preparation method of nanorod material and energy storage application thereof |
| CN113697846B (en) * | 2021-08-05 | 2022-04-29 | 湖北工程学院 | ZnSnO3Preparation method of nanorod material and energy storage application thereof |
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