CN112194187A - Method for synthesizing zinc ferrite spherical nano material by premixed flame - Google Patents
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Abstract
The invention discloses a method for synthesizing a zinc ferrite spherical nano material by premixed flame. The method employs Zn (NO)3)2·6H2O、Fe(NO3)3·9H2O is used as a precursor, stable high-temperature plane flame is formed by adjusting the flow of premixed gas of carrier gas, combustible gas and oxygen and adjusting the distance between a substrate and a nozzle, the atomized precursor is brought into the formed high-temperature flame surface by the carrier gas, and finally ZnFe is successfully prepared2O4Spherical nano material. The preparation method disclosed by the invention is simple in operation steps, low in cost, fast in one-step synthesis, good in product reproducibility, good in product crystallinity and free of impurity phases, the product is uniformly dispersed spherical particles, the particle size is 300-400 nm, and the product is formed by assembling a large number of small particles with the particle size of about 10 nm.
Description
Technical Field
The invention belongs to the technical field of nano material preparation, and relates to a method for synthesizing a zinc ferrite spherical nano material by premixed flame.
Background
Zinc ferrite (ZnFe)2O4) Is a composite semiconductor material with a spinel structure, the spinel structure belongs to a face-centered cubic structure, and each unit cellConsists of 24 metal cations and 32 oxygen ions, and is a cubic structure which takes the oxygen ions as a framework to carry out close accumulation and distributes the metal ions in various gaps. Transition metal cation Zn in spinel structure2+Added into Fe-O crystal lattice, a great deal of oxygen vacancy defects exist in ZnFe due to the difference of Zn and Fe elements in ion size and electronegativity2O4The special structural characteristic of the crystal lattice enables the crystal lattice to have good application advantages in the direction of a gas sensor, and the crystal lattice becomes a good material for detecting reducing gas. For example, nano ZnFe2O4To Cl2，NO2，H2S, ethanol, acetone and the like have high sensitivity. In the spinel structure, the metal ions are subjected to superexchange action through oxygen ions, when ZnFe2O4When the size of the nano-scale crystal reaches the nano-scale, the crystal structure of the nano-scale crystal is changed, so that nano ZnFe is generated2O4The magnetic property of the material is mutated, and the material presents superparamagnetism and can be used as an ideal magnetic wave-absorbing material in a high frequency band. Furthermore, ZnFe2O4As a semiconductor oxide with the forbidden band width of 1.9eV, the semiconductor oxide can generate photoproduction electron-hole pairs under the irradiation of visible light with the wavelength of more than 420nm, and is a semiconductor photocatalyst with high utilization rate of the visible light. ZnFe2O4Due to the special physical and chemical properties, the material has good thermal stability. For example, ZnFe2O4The material has the property of high-temperature semiconductor, is expected to be a preferred matrix material of the inert anode for aluminum, and overcomes the defect of low corrosion resistance. At the same time as transition metal oxide, ZnFe2O4The Li-Zn alloy formed during discharging can provide extra capacitance, so that the performance of the Li-Zn alloy is superior to that of other iron-based bimetallic cathode materials. So far, ZnFe2O4Mainly focused on ZnFe2O4Metal ion doping is carried out to control the crystal defects, or different chemical synthesis methods are adopted to synthesize ZnFe with different shapes2O4And the performance of the structure is improved.
ZnFe2O4The existing chemical synthesis methods mainly comprise a sol-gel method and a chemical synthesis methodPrecipitation, low temperature solid phase reaction, hydrothermal, solvothermal, etc. For example, Qiu et al prepared zinc ferrite nano-film by sol-gel method, and used as photocatalyst to degrade methyl orange under irradiation of xenon lamp, but had disadvantages of expensive raw material and long synthesis period (Jianxun Qiu, Chengyu Wang, et al]Materials Science and Engineering: B,2004,112: 1-4.). Das et al synthesized high crystallinity single phase spinel ZnFe using co-precipitation technique2O4Nanoparticles, but the presence of precipitants may result in local concentrations that are too high and result in agglomeration or insufficiently uniform composition (Vinosha, P.Annie, et al. Synthesis and properties of pigment ZnFe2O4 nanoparticles by surface co-precipitation route [ J.]Optik,2017,134: 99-108). Chu et al prepared ZnFe by hydrothermal method2O4The nano-particles have high gas-sensitive performance to ethanol, but have the defects of difficult control of the nucleation process and the crystal growth process (Xiaongfeng, et al. the gas-sensing properties of the thick film sensors on nano-ZnFe)2O4 prepared by hydrothermal method[J].Materials Science&Engineering B,2006,129: 150-. Preparation of ZnFe by Li et al by low temperature solid phase method2O4The nano particles are respectively calcined at the high temperature of 800 ℃ and 850 ℃ for 3 hours to obtain a high magnetic performance product with the particle size range of 40-60nm, but the defects of large energy consumption, low efficiency and the like (Li F, Wang H, Wang L, et al magnetic properties of ZnFe2O4 nanoparticles produced by a low-temperature solid-state reaction method [ J].Journal of Magnetism&Magnetic Materials,2007,309(2):295-299.). So far, the controlled synthesis of high-quality ZnFe2O4The research on the nano material is still few, and how to further simplify the synthesis process and improve the crystallinity of the product so as to further improve the performance of the product is still needed to be researched.
Disclosure of Invention
In order to overcome the defects of low crystallinity of a product, complicated experimental steps and the like in the existing chemical synthesis method, the invention provides a method for synthesizing a zinc ferrite spherical nano material by premixed flame.
The technical scheme of the invention is as follows:
a method for synthesizing zinc ferrite spherical nano material by premixed flame includes forming stable high temperature plane flame by adjusting premixed gas flow of carrier gas, combustible gas and oxygen and adjusting distance between substrate and nozzle, dissolving precursor in water, atomizing into micron-sized droplets by atomizer, bringing high speed carrier gas into burner, entering high temperature flame area, carrying out a series of homogeneous nucleation and growth, depositing on surface of cooling substrate under action of thermophoresis force, finally obtaining spinel structure ferrite nano material, including the following steps:
the molar ratio of 0.65:2 Zn (NO)3)2·6H2O and Fe (NO)3)3·9H2O as a precursor, Zn (NO)3)2·6H2O and Fe (NO)3)3·9H2Dissolving O in water to form a precursor solution, placing the precursor solution in an atomization device, introducing carrier gas preheated to 200-250 ℃, passing the aerosol formed by atomization through the preheating device, carrying the precursor into a combustor through the carrier gas, then introducing the precursor into a high-temperature flame region, carrying out homogeneous nucleation and growth, and depositing the precursor on the surface of a cooling substrate under the action of thermophoresis force to obtain ZnFe2O4A spherical nanomaterial; the high-temperature flame area is formed by premixed gas of carrier gas, combustible gas ethylene and oxygen.
In the present invention, the carrier gas is a cooling atmosphere and is selected from inert gases such as nitrogen and argon. The flow rate of the carrier gas nitrogen is 9-10 SLPM.
In the invention, the flow rate of the ethylene is 0.65-0.68 SLPM.
In the invention, the flow rate of the oxygen is 3-3.8 SLPM.
In the invention, the temperature of the high-temperature flame area is 1400-1500K.
In the invention, the preheating temperature of the preheating device is set to be 100-130 ℃. The precursor is decomposed in advance due to overhigh temperature, and impurities are generated; the low temperature can cause the aerosol to gather into small liquid drops which enter the wall surface of the combustor through the pipelineUnfavorable to form stable and continuous flame condition, and influence on final ZnFe2O4The formation of the product is not beneficial to preparing the nano material with uniform appearance and pure phase.
In the invention, the distance between the nozzle of the burner and the cooling substrate is 2.8-3 cm.
According to the invention, the cooling substrate is a stainless steel substrate, the inside of the cooling substrate is of a hollowed structure, two symmetrical outlets are formed in two sides of the cooling substrate and are used for being communicated with a circulating cooling water pipeline, and the surface temperature of the water-cooling substrate is ensured to be stabilized at 30-40 ℃ under the action of a circulating water pump.
In the invention, the deposition time is 10-25 min, preferably 10-15 min.
In the present invention, Zn (NO)3)2·6H2O and Fe (NO)3)3·9H2The molar ratio of O is 0.65: 2. under the molar ratio, ZnFe with pure product, uniform appearance and small particle size can be obtained2O4And (3) nano materials. When the molar ratio is higher than the above range, the product has low purity and contains ZnO impurities; at less than this molar ratio, the product is freed from ZnFe2O4In addition, it contains Fe3O4Impurities, destroy the uniqueness of the product.
In the invention, the flow rate of the premixed gas needs to be accurately controlled within a certain range. The flow rate of the carrier gas nitrogen is 9-10 SLPM. When the nitrogen flow is higher than the range, the retention time of the precursor in the flame is too short, the product is amorphous and impurities exist; when the nitrogen flow is lower than the range, the flame plane is unstable, the retention time of the precursor is too long, and the size of the product is increased due to further sintering. The flow rate of combustible gas ethylene is 0.65-0.68 SLPM. When the ethylene gas flow is higher than the range, the original oxygen-enriched flame condition can be destroyed, the oxygen-deficient atmosphere is gradually formed, and the final ZnFe is not facilitated2O4Forming; when the ethylene gas flow is lower than this range, the flame temperature is too low, which is not favorable for the formation of a product with good crystallinity and uniform appearance. The gas flow rate of the oxygen is 3-3.8 SLPM. The gas flow of oxygen is too high, so that the flame plane moves upwards and shakes, even the tempering condition occurs, and the formation of products is not facilitated; the oxygen gas flow is too low, and the oxygen gas flow canResulting in the formation of an oxygen-deficient state, difficult to form the final spherical ZnFe2O4And (3) nano materials.
In order to overcome the defects that the retention time of the precursors in the flame is short, the decomposition reactions of the two precursors are asynchronous, and the preheating of an atomizing device and the setting of the preheating temperature are very critical. Adding Zn (NO)3)2·6H2O and Fe (NO)3)3·9H2The preheating temperature of the O precursor is controlled between 200 ℃ and 250 ℃, which is beneficial to the final spherical ZnFe2O4And (4) forming the nano material. When the preheating temperature is too high, the precursor is decomposed in advance in the atomizing device or the pipeline, so that a large amount of deposited particles are generated in the pipeline connected with the burner, enter a flame area under the action of high-speed carrier gas, generate disturbance on a high-temperature flame plane, and finally produce an amorphous product. When the preheating temperature is too low, the decomposition reactions of the two precursors are asynchronous, and ZnFe is difficult to form after passing through a flame surface2O4Even two separate oxides are formed and further metal ion doping cannot be achieved.
Compared with the prior art, the invention has the following advantages:
(1) the invention successfully prepares ZnFe by adopting a premixing stagnation flame synthesis method2O4Spherical nanoparticles. Preparation of ZnFe2O4The product is uniformly dispersed spherical particles, the particle size is 300-400 nm, a large number of folds are distributed on the surface of the spherical particles, the spherical particles are formed by assembling a large number of small particles with the particle size of about 10nm, and a plurality of mesopores exist among the nano particles, so that the ZnFe can be further increased2O4The specific surface area of the spherical particles provides more active sites of action.
(2) The two solutes contained in the precursor adopted by the invention have similar decomposition temperatures, the difference between the reaction rate and the vapor pressure of the reactant is not large, and the reactants rapidly pass through the flame surface under high-speed carrier gas, so that the purity of the product is good and the product is not interfered by external factors. The prepared product has the element compositions of Zn, Fe and O, the molar ratio of Zn to Fe is approximately 0.5, and the synthesized product is single and has good crystallinity and no impurity phase.
(3) The preparation method has the advantages of simple preparation steps, low cost, one-step rapid synthesis and good reproducibility of the product.
Drawings
FIG. 1 is a process for preparing ZnFe2O4Schematic diagram of a premixing flame synthesis technology device of spherical nano particles;
FIG. 2 shows the spherical nano ZnFe prepared in example 12O4XRD pattern of (a);
FIG. 3 is an XRD pattern of the products obtained in comparative examples 1, 2 and 3;
FIG. 4 shows the spherical nano ZnFe prepared in example 12O4SEM picture of (1);
FIG. 5 shows the spherical nano ZnFe prepared in example 12O4A TEM image of (a).
Detailed Description
The invention is further illustrated by the following examples and figures.
Preparation of ZnFe2O4The apparatus for premixed flame synthesis of nanomaterials is shown in fig. 1. The device mainly comprises an air supply system, a gas flow control system, a circulating water cooling system, a preheating heating belt, an air heating pipe, an atomizing device, a circuit control system and the like.
The gas supply system is formed by connecting oxygen, nitrogen, ethylene and corresponding pipelines, and the gas flow control system is used for accurately controlling the gas flowing out. The preheating heating belt and the air heating pipe belong to a preheating device, and are required to be set to the optimal temperature before the experiment is started until the preheating is finished. The circulating water cooling system is connected with the stainless steel hollow substrate, so that the temperature before the start of the experiment and in the experiment process is ensured to be 30-40 ℃. Putting the precursor prepared according to the proportion into an atomizing device container, atomizing the precursor into micron-sized liquid drops, then bringing the liquid drops into a high-temperature flame zone by carrier gas, and finally obtaining ZnFe on a cooling substrate through a series of decomposition, nucleation and growth2O4And (3) nano materials.
Example 1
ZnFe2O4Preparation of spherical nano material
Mixing 2g ofZn(NO3)2·6H2O and 8.08g Fe (NO)3)3·9H2Adding O (the molar ratio is 0.65:2) into 50mL of deionized water, stirring and mixing uniformly, placing the mixture in a magnetic stirrer at room temperature, stirring for 20-30 min at a speed of 250r/min, and pouring the mixture into an atomization device after stirring. And opening a circulating water cooling system, checking whether the water quantity of the water pump is sufficient and the liquid inlet condition of the liquid in the pipeline, and ensuring the cooling effect of the water-cooling substrate. The preheating device of the burner and the preheating heating belt of the pipeline are respectively arranged at 130 ℃ and 100 ℃, the temperature of the air heating pipe is arranged at 250 ℃, and the experimental device is preheated. And opening a nitrogen valve after preheating is finished, checking the airtightness of the whole gas circuit, observing whether the numerical value of the Dwyer digital display pressure gauge suddenly drops, simultaneously increasing the flow of a protective gas circuit, and emptying residual moisture in the combustor and residual air in the pipeline. Adjusting the distance between a nozzle of the burner and the substrate to be 2.8-3 cm, controlling the flow rate of the carrier gas to be 9-10SLPM, controlling the flow rate of the ethylene to be 0.65-0.68 SLPM, and controlling the flow rate of the oxygen to be 3-3.8 SLPM. And after the parameters are stable, adjusting stable plane flame at 1400-1500K. And correspondingly fine-adjusting according to the flame condition, opening the atomizer and adjusting carrier gas to bring the precursor into the burner after the flame is stabilized for 3min and under the conditions of no shaking, extinguishing and tempering, observing the flame change condition, adjusting the atomizer to a proper gear until the flame surface has no layering phenomenon, and ensuring that the flame color reaction is obvious and uniform. After passing through a high-temperature flame region, a series of reactions occur, and after 15min of deposition, ZnFe is finally collected on a cooling substrate2O4And (3) nano materials.
FIG. 2 shows the spherical nano ZnFe prepared in example 12O4The XRD pattern of (A) corresponds to each characteristic peak of the standard cardstock JCPDS #73-1963, which shows that the purity of the product is higher and the crystallinity is better.
FIG. 4 shows the spherical nano ZnFe prepared in example 12O4SEM image of (d). ZnFe2O4The product is uniformly dispersed spherical particles, and the particle size is 300-400 nm.
FIG. 5 shows the spherical nano ZnFe prepared in example 12O4A TEM image of (a). Spherical particles ofA large number of small particles with the particle size of about 10nm are assembled, and a plurality of mesopores exist among the nano particles, which is beneficial to further increasing the ZnFe2O4The specific surface area of the spherical particles provides more active sites of action.
Comparative example 1
Compared with example 1, the difference is Zn (NO)3)2·6H2O and Fe (NO)3)3·9H2The molar ratio of O was 1:2, and other experimental conditions were unchanged. As shown in fig. 3, a ZnO impurity peak was present.
Comparative example 2
Compared with example 1, the difference is Zn (NO)3)2·6H2O and Fe (NO)3)3·9H2The molar ratio of O was 0.4:2, and other experimental conditions were unchanged, as shown in fig. 3, there was a peak of impurities.
Comparative example 3
The difference from example 1 is that the ethylene flow rate was changed to 0.63SLPM, and the other experimental conditions were not changed. As shown in fig. 3, a ZnO impurity peak was present.
Claims (10)
1. The method for synthesizing the zinc ferrite spherical nano material by premixed flame is characterized by comprising the following steps of:
the molar ratio of 0.65:2 Zn (NO)3)2·6H2O and Fe (NO)3)3·9H2O as a precursor, Zn (NO)3)2·6H2O and Fe (NO)3)3·9H2Dissolving O in water to form a precursor solution, placing the precursor solution in an atomization device, introducing carrier gas preheated to 200-250 ℃, passing the aerosol formed by atomization through the preheating device, carrying the precursor into a combustor through the carrier gas, then introducing the precursor into a high-temperature flame region, carrying out homogeneous nucleation and growth, and depositing the precursor on the surface of a cooling substrate under the action of thermophoresis force to obtain ZnFe2O4A spherical nanomaterial; the high-temperature flame area is formed by premixed gas of carrier gas, combustible gas ethylene and oxygen.
2. The method of claim 1 wherein the carrier gas is a cooling atmosphere selected from the group consisting of nitrogen and argon.
3. The method of claim 2, wherein the flow rate of the carrier gas nitrogen is 9-10 SLPM.
4. The method of claim 1, wherein the ethylene flow rate is 0.65 to 0.68 SLPM.
5. The method of claim 1, wherein the flow rate of the oxygen is 3 to 3.8 SLPM.
6. The method of claim 1, wherein the high temperature flame zone has a temperature of 1400-1500K.
7. The method according to claim 1, wherein the preheating temperature of the preheating device is set to 100 to 130 ℃.
8. The method according to claim 1, wherein the cooling substrate is a stainless steel substrate, the temperature of the surface of the substrate is stabilized at 30 to 40 ℃, and the distance between the burner nozzle and the cooling substrate is 2.8 to 3 cm.
9. The method of claim 1, wherein the deposition time is 10 to 25 min.
10. The method according to claim 1, wherein the deposition time is 10 to 15 min.
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| CN113181856A (en) * | 2021-05-08 | 2021-07-30 | 东南大学 | Device and method for synthesizing nano particles by simulating zero-microgravity flame with assistance of magnetic field |
| CN115305347A (en) * | 2022-08-27 | 2022-11-08 | 苏州金之翼新材料科技有限公司 | Method for preparing zinc ferrite from neodymium iron boron waste |
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