CN109455766B - Superfine zinc ferrite nano-particles, preparation method and gas-sensitive application thereof - Google Patents
Superfine zinc ferrite nano-particles, preparation method and gas-sensitive application thereof Download PDFInfo
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- 229910001308 Zinc ferrite Inorganic materials 0.000 title claims abstract description 101
- WGEATSXPYVGFCC-UHFFFAOYSA-N zinc ferrite Chemical compound O=[Zn].O=[Fe]O[Fe]=O WGEATSXPYVGFCC-UHFFFAOYSA-N 0.000 title claims abstract description 99
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000000203 mixture Substances 0.000 claims abstract description 24
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 claims abstract description 15
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002243 precursor Substances 0.000 claims abstract description 15
- 238000000137 annealing Methods 0.000 claims abstract description 13
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- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 5
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- 239000011701 zinc Substances 0.000 claims description 5
- QZRHHEURPZONJU-UHFFFAOYSA-N iron(2+) dinitrate nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QZRHHEURPZONJU-UHFFFAOYSA-N 0.000 claims description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SZQUEWJRBJDHSM-UHFFFAOYSA-N 0.000 claims description 3
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- 239000004065 semiconductor Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- QGJOPFRUJISHPQ-NJFSPNSNSA-N carbon disulfide-14c Chemical compound S=[14C]=S QGJOPFRUJISHPQ-NJFSPNSNSA-N 0.000 description 2
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- 238000003837 high-temperature calcination Methods 0.000 description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 2
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- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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Abstract
The invention discloses an ultrafine zinc ferrite nanoparticle, a preparation method and gas-sensitive application thereof, wherein a zinc ferrite precursor is prepared for annealing treatment to prepare the ultrafine zinc ferrite nanoparticle, the spherical diameter of the ultrafine zinc ferrite nanoparticle is 8-10nm, and the specific surface area of the ultrafine zinc ferrite nanoparticle is 70-90m2(ii) in terms of/g. Dispersing superfine zinc ferrite nanoparticles in a small amount of ethanol, brushing the mixture on a flat electrode by using a brush, drying the dried mixture in an oven at the temperature of between 60 and 80 ℃, and using the dried mixture in a gas-sensitive test. The gas-sensitive material can realize uniform size, good dispersibility, excellent gas-sensitive property to nitrogen dioxide gas at lower working temperature, and can be used for gas-sensitive research of nitrogen dioxide and harmful gases thereof.
Description
Technical Field
The invention relates to a synthesis technology of a semiconductor gas sensor, in particular to superfine zinc ferrite nano particles, a preparation method and gas-sensitive application thereof.
Background
Semiconductor type gas sensors have been widely used for safety, medical testing, food safety, and particularly for the detection of toxic gases, due to their good stability, good selectivity, low cost, and portability. The gas sensor is a sensing device for converting information such as components and contents of gas into electrical information, and can be used for qualitatively or quantitatively detecting target gas. With the development of economic society, the environmental pollution problem caused by the industrialized era is increasingly prominent, and especially the problem of air quality reduction is increasingly serious. For example, the fog and haze weather appearing in recent years is severe weather caused by air pollution, so that the problem that flammable, explosive, toxic and harmful gases are accurately and reliably monitored or automatic control is implemented is urgently needed to be solved. However, the sensitivity, response time, selectivity, operating temperature and long-term stability of the semiconductor gas sensor are high, which limits further application of the semiconductor gas sensor, and the gas-sensitive performance of the gas sensor not only hinders commercial application of the semiconductor gas sensor, but also makes it more difficult to detect gases which are difficult to detect per se, so that the synthesis of a gas-sensitive material with excellent gas-sensitive performance has important significance.
In recent years, spinel zinc ferrite (ZnFe2O4) has been gaining attention in many fields as an important functional n-type semiconductor due to its good chemical stability and good thermal stability. Of course, neat or modified zinc ferrites have been used as photovoltaic materials and surface catalysts, respectively, for light-driven water splitting and photocatalytic degradation of contaminants. Although zinc ferrite exhibits many excellent chemical and physical properties at reversible potentials, such as lower photoelectric current, higher charge transfer efficiency, there are fewer reports in gas sensors in addition to the high sensitivity of acetone sensors. To date, sensors based on zinc ferrite production have found little use in nitrogen dioxide sensing.
Disclosure of Invention
The invention aims to provide superfine zinc ferrite nanoparticles, a preparation method and gas-sensitive application thereof.
The purpose of the invention is realized by the following technical scheme:
the superfine zinc ferrite nano-particles comprise zinc ferrite superfine nano-particles, wherein the ball diameter of the zinc ferrite superfine nano-particles is 8-10nm, and the specific surface area of the zinc ferrite superfine nano-particles is 70-90m2/g。
The preparation method of the superfine zinc ferrite nano-particles, provided by the invention, is used for preparing a zinc ferrite precursor for annealing treatment to prepare the superfine zinc ferrite nano-particles, and specifically comprises the following steps:
step A, firstly weighing zinc nitrate hexahydrate (Zn (NO)3)26H2O 0.1782-0.5346 g, iron nitrate nonahydrate (Fe (NO)3)39H2O) 0.4848-1.4544 and 30-90 ml of ethanol solution are mixed, ammonia water is added into the mixed solution after the mixture is uniformly mixed, the pH value of the solution is adjusted to 9-11, the solution is placed on a magnetic stirrer to be continuously stirred for 10-60 min at the rotating speed of 600r/min, then the mixed solution is placed in a water bath at the temperature of about 20 ℃ and continuously subjected to ultrasonic treatment for 10-60 min, then the mixed solution is transferred to a high-pressure reaction kettle with a polytetrafluoroethylene lining, and the high-pressure reaction kettle is placed in an oven at the temperature of 150-230 ℃ to react for 6-24H.
B, removing the supernatant of the mixed solution, washing the remaining mixture with 20-80 ml of ethanol solution, performing ultrasonic treatment for 10-30 min until the mixture is uniformly dispersed, centrifuging the mixture in a centrifuge with the rotating speed of 6000-10000 r/min for 5-10 min, repeating the washing and centrifuging process for 3 times, and drying the mixture with the supernatant removed in an oven at the temperature of 60 ℃ for 12-48 h to obtain a zinc ferrite nanoparticle precursor;
and C, annealing the superfine zinc ferrite nanoparticle precursor obtained by drying at 300-700 ℃ for 1-4h in air, wherein the heating rate is 1-10 ℃/min, and thus obtaining the superfine zinc ferrite nanoparticles.
According to the gas-sensitive application of the superfine zinc ferrite nano-particles, the superfine zinc ferrite nano-particles are dispersed in a small amount of ethanol, then the superfine zinc ferrite nano-particles are brushed on a flat electrode by a brush, dried in the air and dried in a drying oven at the temperature of 60-80 ℃, and the superfine zinc ferrite nano-particles are used during gas-sensitive test.
According to the technical scheme provided by the invention, the superfine zinc ferrite nanoparticles, the preparation method and the gas-sensitive application thereof provided by the embodiment of the invention have the advantages that the prepared zinc ferrite is used as a precursor, and the granular zinc ferrite nanoparticles are prepared through high-temperature calcination annealing and other procedures, so that the uniform size and good dispersibility can be realized, and the superfine zinc ferrite nanoparticles have excellent gas-sensitive characteristics on nitrogen dioxide gas at a lower working temperature.
Drawings
FIG. 1 is an XRD picture of ultrafine zinc ferrite nanoparticles provided by an embodiment of the invention;
fig. 2 is a transmission electron microscope photograph of the ultra-fine zinc ferrite nanoparticles provided in the embodiment of the present invention, in fig. 2, (a), (b), (c) respectively illustrate the observation of the ultra-fine zinc ferrite nanoparticles, and (d) performs mapping composition analysis on the agglomerated ultra-fine zinc ferrite nanoparticles;
FIG. 3 is a photograph of the transmission of a zinc ferrite sample prepared by an example of the present invention, and (a) (b) in FIG. 3 are photographs of the transmission of a zinc ferrite sample prepared at annealing temperatures of 300 and 700 deg.C, respectively;
FIG. 4 shows the gas sensitivity test of zinc ferrite nanoparticles at calcination temperatures of 300,500 and 700 ℃ for nitrogen dioxide (R) at 75,100,125,150,175 and a working temperature of 200 ℃ for examples of the inventiongas/Rair) -a time(s) curve;
FIG. 5 is a gas sensitivity test Response (Rg/Rair) -time(s) curve of the ultrafine zinc ferrite nanoparticles prepared by calcination at 500 ℃ in an air atmosphere at a working temperature of 125 ℃ for nitrogen dioxide in accordance with an embodiment of the present invention;
fig. 6 is a Response (Rg/Rair) -time(s) curve of gas sensitivity test of the ultrafine zinc ferrite nanoparticles prepared by calcination at 500 ℃ in air atmosphere at 125 ℃ for formaldehyde, hydrogen sulfide, ammonia gas, carbon disulfide, sulfur dioxide and nitrogen dioxide.
Detailed Description
The embodiments of the present invention will be described in further detail below. Details which are not described in detail in the embodiments of the invention belong to the prior art which is known to the person skilled in the art.
The invention discloses a superfine zinc ferrite nano-particle, a preparation method and gas-sensitive application thereof, wherein the preferable specific implementation mode is as follows:
the superfine zinc ferrite nanoparticles comprise zinc ferrite superfine nanoparticles, wherein the ball diameter of the zinc ferrite superfine nanoparticles is 8-10nm, and the specific surface area of the zinc ferrite superfine nanoparticles is 70-90m2/g。
The preparation method of the superfine zinc ferrite nano-particles comprises the following steps of preparing a zinc ferrite precursor, and annealing the zinc ferrite precursor to obtain the superfine zinc ferrite nano-particles:
step A, firstly weighing zinc nitrate hexahydrate (Zn (NO)3)26H2O 0.1782-0.5346 g, iron nitrate nonahydrate (Fe (NO)3)39H2O) 0.4848-1.4544 and 30-90 ml of ethanol solution are mixed, ammonia water is added into the mixed solution after the mixture is uniformly mixed, the pH value of the solution is adjusted to 9-11, the solution is placed on a magnetic stirrer to be continuously stirred for 10-60 min at the rotating speed of 600r/min, then the mixed solution is placed in a water bath at the temperature of about 20 ℃ and continuously subjected to ultrasonic treatment for 10-60 min, then the mixed solution is transferred to a high-pressure reaction kettle with a polytetrafluoroethylene lining, and the high-pressure reaction kettle is placed in an oven at the temperature of 150-230 ℃ to react for 6-24H.
B, removing the supernatant of the mixed solution, washing the remaining mixture with 20-80 ml of ethanol solution, performing ultrasonic treatment for 10-30 min until the mixture is uniformly dispersed, centrifuging the mixture in a centrifuge with the rotating speed of 6000-10000 r/min for 5-10 min, repeating the washing and centrifuging process for 3 times, and drying the mixture with the supernatant removed in an oven at the temperature of 60 ℃ for 12-48 h to obtain a zinc ferrite nanoparticle precursor;
and C, annealing the superfine zinc ferrite nanoparticle precursor obtained by drying at 300-700 ℃ for 1-4h in air, wherein the heating rate is 1-10 ℃/min, and thus obtaining the superfine zinc ferrite nanoparticles.
The molar ratio of zinc nitrate hexahydrate to ferric nitrate nonahydrate after being dissolved in an ethanol solution is 1-2: 2-4, the mass concentration of the ethanol solution is 75%, the mass concentration of ammonia water (NH 3. H2O) is 25.0-28.0%, and the mixed solution is placed in an oven at 180 ℃ for reaction for 12 hours.
The mass concentration of the ethanol solution is 75%.
The zinc ferrite precursor is placed in an annealing furnace at 500 ℃ for reaction for 2 hours in the air atmosphere, and the heating rate is 2 ℃/min.
In the gas-sensitive application of the superfine zinc ferrite nano-particles, the superfine zinc ferrite nano-particles are dispersed in a small amount of ethanol, then are brushed on a flat electrode by a brush, are dried in an oven at 60-80 ℃ after being dried, and are used in a gas-sensitive test.
According to the superfine zinc ferrite nano-particles, the preparation method and the gas-sensitive application thereof, the prepared zinc ferrite is used as a precursor, and the granular zinc ferrite nano-particles are prepared through procedures of high-temperature calcination annealing and the like, so that the superfine zinc ferrite nano-particles are uniform in size and good in dispersity, and have excellent gas-sensitive property on nitrogen dioxide gas at a lower working temperature.
The superfine zinc ferrite nano-particles prepared by the invention have the following advantages:
(1) the superfine zinc ferrite nano-particles provided by the invention can be directly used as gas-sensitive materials and used for gas-sensitive research of nitrogen dioxide and harmful gases thereof.
(2) The superfine zinc ferrite nano-particles provided by the invention have larger specific surface area, increase the contact area between gas and materials and are beneficial to gas detection.
(3) The preparation method of the superfine zinc ferrite nano-particles provided by the invention only needs common equipment in a laboratory, does not need special equipment, and has simple process and easy operation.
(4) The invention can prepare the superfine zinc ferrite nano-particles with uniform size and good monodispersity.
In order to more clearly show the technical scheme and the technical effects thereof provided by the present invention, the following detailed description of the ultrafine zinc ferrite nanoparticles provided by the present invention, the preparation method thereof and the application thereof are provided by specific examples.
Example 1
The preparation method of the superfine zinc ferrite nano-particles comprises the following steps:
step a1, zinc nitrate hexahydrate (Zn (NO) is weighed out first3)26H2O)0.3564g, iron nitrate nonahydrate (Fe (NO)3)39H2O)0.9696g of the mixed solution is mixed with 60ml of ethanol solution, ammonia water is added into the mixed solution dropwise after the mixture is uniformly mixed, the pH value of the solution is adjusted to 10, the solution is placed on a magnetic stirrer to be continuously stirred for 30min at the rotating speed of 600r/min, then the mixed solution is placed in a water bath at the temperature of about 20 ℃ and continuously subjected to ultrasonic treatment for 30min, and then the mixed solution is transferred to a polytetrafluoroethylene liningAnd (4) placing the mixture in a pressure reaction kettle and an oven at 180 ℃ for reaction for 12 hours.
B1, removing the supernatant of the mixed solution, washing the rest mixture with 50ml of ethanol solution, performing ultrasonic treatment for 10min until the mixture is uniformly dispersed, centrifuging the mixture in a centrifuge with the rotation speed of 8000r/min for 5min, repeating the washing and centrifuging process for 3 times, and drying the mixture with the supernatant removed in an oven at 60 ℃ for 24h to obtain the ultrafine zinc ferrite nanoparticles; the molar ratio of zinc nitrate hexahydrate to ferric nitrate nonahydrate after being dissolved in an ethanol solution is 1:2, the mass fraction of the ethanol solution is 75% of absolute ethanol, and the mass fraction of ammonia water is 25-28%.
And c1, carrying out centrifugal separation and centrifugal cleaning treatment on the prepared superfine zinc ferrite nano-particles, wherein the rotating speed of the centrifugal separation and cleaning treatment is 8000r/min, then obtaining centrifugal precipitates, and drying in a drying oven at 60 ℃ to obtain the zinc ferrite nano-particles.
D1, annealing the superfine zinc ferrite nano-particles obtained by drying at 500 ℃ in the air for 2h, wherein the heating rate is 2 ℃/min, so as to prepare the superfine zinc ferrite nano-particles;
appearance observation and performance detection:
the appearance observation and the performance detection are carried out on the superfine zinc ferrite nanoparticle sample prepared in the embodiment 1 of the invention, so that the following results are obtained:
(1) XRD is adopted to analyze and determine a phase, and a transmission electron microscope and mapping are adopted to analyze the appearance of the prepared superfine zinc ferrite nano particle sample, so that an XRD picture shown in figure 1 and a transmission electron microscope picture shown in figure 2 are obtained. From the XRD pattern, (111), (220), (311), (222), (400), (422), (511) and (440) are all crystal planes corresponding to the peak positions of the characteristic crystal planes of zinc ferrite, and the obtained sample is proved to be zinc ferrite, and from figure 2a, our sample is indeed in the form of small particles with a particle diameter of about 8-10 nm. The selected area diffraction pattern can be seen to be composed of concentric circular tubes with different sizes, and different circular rings correspond to different crystal faces of the zinc ferrite, so that the formation of a zinc ferrite phase is further proved.
(2) 2a, b, c are further observed by transmission electron microscopy on zinc ferrite nanoparticles obtained by calcination at a temperature of 500 ℃ and it can be seen that the zinc ferrite is composed of small single-crystal particles, the size of which is about 8-10nm, and the morphology is such that the specific surface area of the zinc ferrite nanoparticles is larger; FIG. 2d is mapping composition analysis of the agglomerated ultra-fine zinc ferrite nanoparticles, which shows that the nanoparticles are composed of Fe and Zn elements, further proving the formation of the zinc ferrite phase.
(3) Fig. 3a and b are transmission images of zinc ferrite samples prepared at annealing temperatures of 300 and 700 c, respectively, and it can be seen that as the annealing temperature is increased, zinc ferrite particles are gradually grown to cause polymerization between the zinc ferrite particles.
(4) The superfine zinc ferrite nano particles prepared by the method are used as gas-sensitive materials, ethanol is used for mixing, a brush is used for coating on a planar electrode, the drying is carried out at 60 ℃, the aging is carried out for 48 hours in an aging table, and then the gas-sensitive detection is carried out, wherein a graph shown in figure 4 shows that the superfine zinc ferrite nano particles obtained by calcining a zinc ferrite precursor at 500 ℃ show excellent gas-sensitive performance to nitrogen dioxide at the working temperature of 125 ℃ when the zinc ferrite nano particles are subjected to gas-sensitive test Response (Rg/Rair) -time(s) at the calcining temperatures of 300,500 and 700 ℃ respectively.
(5) Fig. 5 is a Response (Rg/Rair) -time(s) curve of gas sensitivity test of the superfine zinc ferrite nano-particles prepared by calcining at 500 ℃ in air atmosphere to nitrogen dioxide at 125 ℃ working temperature, and it can be seen that the superfine zinc ferrite nano-particles show excellent gas sensitivity to nitrogen dioxide.
(6) Fig. 6 is a gas sensitivity test Response (Rg/Rair) -time(s) curve of the ultrafine zinc ferrite nanoparticles prepared by calcination at 500 ℃ in an air atmosphere at a working temperature of 125 ℃ for formaldehyde, hydrogen sulfide, ammonia gas, carbon disulfide, sulfur dioxide and nitrogen dioxide, and it can be seen that the ultrafine zinc ferrite nanoparticles exhibit excellent selectivity for nitrogen dioxide.
In conclusion, the prepared gas sensor has larger specific surface area, superior selectivity and excellent gas-sensitive performance at lower working temperature.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (1)
1. A preparation method of superfine zinc ferrite nano particles is characterized by comprising the following steps:
the diameter of the superfine zinc ferrite nano-particle is 8-10nm, and the specific surface area is 70-90m2/g；
The method for preparing the superfine zinc ferrite nano-particle precursor comprises the following steps:
step A, firstly weighing zinc nitrate hexahydrate (Zn (NO)3)26H2O 0.1782-0.5346 g, iron nitrate nonahydrate (Fe (NO)3)39H2O) 0.4848-1.4544 g of the mixed solution is mixed with 30-90 ml of ethanol solution, ammonia water is dripped into the mixed solution after the mixture is uniformly mixed, the pH value of the solution is adjusted to 9-11, the mixed solution is placed on a magnetic stirrer to be continuously stirred for 10-60 min at the rotating speed of 600r/min, then the mixed solution is placed in a water bath at the temperature of 20 ℃ and continuously subjected to ultrasonic treatment for 10-60 min, then the mixed solution is transferred to a high-pressure reaction kettle with a polytetrafluoroethylene lining, and the high-pressure reaction kettle is placed in an oven at the temperature of 180 ℃ to react for 12H;
b, removing the supernatant of the mixed solution, washing the remaining mixture with 20-80 ml of ethanol solution, performing ultrasonic treatment for 10-30 min until the mixture is uniformly dispersed, centrifuging the mixture in a centrifuge with the rotating speed of 6000-10000 r/min for 5-10 min, repeating the washing and centrifuging process for 3 times, and drying the mixture with the supernatant removed in an oven at the temperature of 60 ℃ for 12-48 h to obtain the superfine zinc ferrite nanoparticle precursor;
c, annealing the dried superfine zinc ferrite nanoparticle precursor for 2 hours at 500 ℃ in the air, wherein the heating rate is 2 ℃/min, and thus the superfine zinc ferrite nanoparticles are prepared;
in the step A, the molar ratio of zinc nitrate hexahydrate to ferric nitrate nonahydrate dissolved in an ethanol solution is 1-2: 2-4, the mass concentration of the ethanol solution is 75%, and the mass concentration of ammonia water (NH 3. H2O) is 25.0-28.0%;
in the step B, the mass concentration of the ethanol solution is 75 percent;
the superfine zinc ferrite nano particles are dispersed in a small amount of ethanol, then brushed on a flat electrode by a brush, dried in the air and dried in a drying oven at the temperature of 60-80 ℃, and used in the nitrogen dioxide gas-sensitive test.
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| CN107364897A (en) * | 2017-08-17 | 2017-11-21 | 大连理工大学 | A kind of preparation method of ferrous acid zinc nano material |
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| Ultrasonic cavitation assisted solvothermal synthesis of superparamagnetic zinc ferrite nanoparticle;Sireenart Surinwong等;《Particuology》;20131231;第588-593页 * |
| ZnFe2O4 nanoparticles: Synthesis，characterization，and enhanced gas sensing property for acetone;Jie Zhang等;《Sensors and Actuators B：Chemical》;20150620;第55-62页 * |
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