CN111235625B - Iron oxide single crystal nano spherical particle and molten salt method synthesis method thereof - Google Patents

Iron oxide single crystal nano spherical particle and molten salt method synthesis method thereof Download PDF

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CN111235625B
CN111235625B CN202010070422.1A CN202010070422A CN111235625B CN 111235625 B CN111235625 B CN 111235625B CN 202010070422 A CN202010070422 A CN 202010070422A CN 111235625 B CN111235625 B CN 111235625B
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iron oxide
single crystal
oxide single
molten salt
nano
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CN111235625A (en
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娄正松
张凯
秦佳佳
徐晨晰
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Changzhou Youna New Material Technology Co ltd
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Jiangsu University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B9/00—Single-crystal growth from melt solutions using molten solvents
    • C30B9/04—Single-crystal growth from melt solutions using molten solvents by cooling of the solution
    • C30B9/08—Single-crystal growth from melt solutions using molten solvents by cooling of the solution using other solvents
    • C30B9/12—Salt solvents, e.g. flux growth
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/16—Oxides
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape

Abstract

The invention discloses an iron oxide single crystal spherical nano-particle and a molten salt synthesis method thereof, which comprises the steps of firstly, uniformly mixing iron salt, KCl and LiCl according to a certain amount ratio, then, roasting at high temperature, soaking in distilled water for desalting, carrying out suction filtration, washing and drying to obtain a product, wherein the product is a monodisperse iron oxide single crystal spherical nano-particle, and the particle size is 100-1000 nm. The method disclosed by the invention has the advantages of wide raw material source, low preparation cost, simple process, environmental friendliness, short time consumption, low energy consumption and strong controllability, and provides a material basis for further expanded use of the iron oxide nanoparticles.

Description

Iron oxide single crystal nano spherical particle and molten salt method synthesis method thereof
Technical Field
The invention relates to the technical field of nano materials, in particular to iron oxide single crystal nano spherical particles and a molten salt method synthesis method thereof.
Background
Iron oxide material, the most common iron oxide in nature, is an important inorganic compound and also a semiconductor material with a forbidden band width of 2.2 eV, unit cell parameters a =0.5043 a, c =1.375 a, belonging to the trigonal system, approximately as close-packed hexagonal, with O being the most common in nature2-Ion deposition near HCP, Fe3+The ions occupy the oxygen ion octahedral voids, but fill only 2/3 of the voids. The iron oxide nano particles belong to semiconductor materials, have strong absorption in a visible light region, and have the characteristics of high capacity, high safety, abundant resources and environmental friendliness, so that the iron oxide nano particles are widely applied to photocatalysis, photosensitive sensors and photoelectric instruments.
Nanomaterials generally refer to materials that have at least one dimension in the three-dimensional range that is on the order of nanometers and that have high-density interfacial phase components. Due to the characteristics of quantum size effect, surface effect, small size effect, macroscopic quantum effect and the like, the nano particles present many exotic physical and chemical properties and present many basic characteristics different from the conventional size materials. The nanocrystallization of the material can improve the electrochemical activity of the ferric oxide, improve the thoroughness of the reaction degree and contribute to improving the cycling stability of the material. The iron oxide nano material researched at present comprises a one-dimensional nano structure, a mesoporous nano structure, a porous microsphere and the like, and has wide application in the fields of plastic products, coatings, catalysts, magnetic materials, medicine and bioengineering due to the characteristics of stable chemical properties and high catalytic activity of the iron oxide nano material.
Fe2O3As a typical N-type semiconductor, it is one of the most promising functional oxides due to its advantages of non-toxicity, high stability and low cost. alpha-Fe2O3Has a three-side phase structure and is common iron oxide in nature. O in its structure2-Ion deposition near HCP, Fe3+The ions occupy oxygen ion octahedral voids. Fe2O3The lithium ion battery cathode material has the advantages of high capacity, high safety, abundant resources, low price and environmental friendliness. However, the application of iron oxide to the negative electrode of a lithium battery is limited in three ways. First, its electrochemical activity is significantly affected by its size and morphology. Only when the size of the material is reduced to the nanometer level, the material shows good electrochemical activity. Also, different nanotopography also affects their electrochemical performance. Secondly, iron oxide is an n-type semiconductor, and has poor conductivity, thus affecting the performance of the iron oxide under high current. Third, iron oxide undergoes large volume changes during cycling, resulting in pulverization of the material and capacity fade. In response to the above problems, the nano-sizing of materials is undoubtedly an effective means for improving the properties thereof. Firstly, the electrochemical activity of the ferric oxide can be improved by the nano material. The nanometer size can shorten the migration path of lithium ions and improve the thoroughness of the reaction degree, thereby being beneficial to improving the electrochemical cycling stability of the ferric oxide. Secondly, the small size and large specific surface of the nano material are beneficial to the transfer of lithium ions and charges, and can improve the charge of the material under large currentRate capability under discharge. Finally, the nano material has better deformation bearing capacity relative to a macroscopic material, is not easy to pulverize, and is also beneficial to improving the cycling stability of the material. However, the synthesis method of the iron oxide nanoparticles in the prior art has the problems of high process cost, poor product performance, poor size controllability, non-uniform morphology, poor dispersibility and the like.
Therefore, there is a need to develop a method for synthesizing iron oxide nano spherical particles with good size controllability, uniform morphology, good dispersibility and easy mass synthesis.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and provides iron oxide single crystal nano spherical particles and a molten salt method synthesis method thereof, which have the advantages of simple synthesis process, easiness for large-scale preparation, good size controllability, uniform appearance and good dispersibility of products, and wide market application prospect in the fields of photocatalysis, photosensitive sensors and photoelectric instruments.
The technical scheme of the invention is as follows: a molten salt method for synthesizing iron oxide single crystal nano spherical particles comprises the following steps:
(1) uniformly mixing iron salt, KCl and LiCl;
(2) collecting the mixture in an alumina crucible, putting the alumina crucible into a muffle furnace, heating, roasting and naturally cooling;
(3) soaking the product after reaction in deionized water to remove salt, and performing suction filtration to obtain a reddish brown solid;
(4) and taking the obtained reddish brown solid out of a centrifugal tube, centrifugally washing the solid for a plurality of times by using deionized water, and drying the solid in vacuum to obtain the spherical ferric oxide nano-particles.
Further, in step 1, the mass ratio of the iron salt, KCl and LiCl is 2: 50 x: 20 x; wherein 0.2< x < 2.2.
Further, in step 1, the iron salt includes one or more of ferric nitrate, ferrous acetate, ferrous oxalate, ferric oxalate and ferrous carbonate.
Further, in step 1, the three materials were uniformly mixed by grinding and mixing using an agate mortar.
Further, in the step 2, the temperature is raised to 530-800 ℃ at the speed of 5 ℃/min for 2-6 h; the reaction temperature is lower than 530 ℃, or the reaction time is lower than 2 hours, the solid mixture can not be completely reacted and can not be completely converted into spherical iron oxide nano-particles; if the reaction temperature in step 2 is higher than 800 deg.c, the solid mixture is converted into iron oxide nanoparticles having large and non-uniform particles.
Further, in the step 4, the temperature for vacuum drying is 40-80 ℃.
The iron oxide single crystal nano-particles prepared by the method are spherical, and the particle size is 100-1000 nm.
The invention has the beneficial effects that:
the invention discloses a ferric oxide single crystal nanometer spherical particle and a molten salt method synthesis method thereof, wherein the preparation method comprises the steps of uniformly mixing ferric salt, KCl and LiCl according to a certain amount ratio of substances, roasting at high temperature, soaking in distilled water for desalting, filtering, washing, and drying to obtain the product, namely the spherical ferric oxide single crystal nanometer particle; the method has the advantages of wide raw material source, low preparation cost, simple process, environmental friendliness, short time consumption, low energy consumption, excellent product performance and strong controllability, and widens the market application prospect of the iron oxide nanoparticles in photocatalysis, photosensitive sensors and optoelectronic instruments.
Drawings
FIG. 1 is an X-ray diffraction pattern of spherical iron oxide nanoparticles prepared in example 1 of the present invention;
FIG. 2 is a scanning electron microscope photograph of spherical iron oxide nanoparticles prepared in example 1 of the present invention;
FIG. 3 is an enlarged view of a portion of FIG. 2;
FIG. 4 is a high-resolution TEM image of spherical iron oxide nanoparticles prepared in example 1 of the present invention;
FIG. 5 is Fe of spherical iron oxide nanoparticles prepared in example 1 of the present invention2O3The rate capability and the efficiency-specific capacity curve of charging and discharging;
fig. 6 is a scanning electron microscope photograph of spherical iron oxide nanoparticles prepared in example 2 of the present invention.
Detailed Description
The following examples further illustrate the present invention but are not to be construed as limiting the invention. Modifications and substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit of the invention.
Example 1
Mixing Fe (NO)3)3KCl and LiCl are mixed according to the mass ratio of 2: 100: 40, and are ground by using an agate mortar to achieve the effect of uniform mixing; collecting the mixture in an alumina crucible, putting the alumina crucible into a muffle furnace, heating to 540 ℃ at the speed of 5 ℃/min, roasting for 4 hours, and naturally cooling; soaking the product after reaction in deionized water to remove salt, and performing suction filtration to obtain a reddish brown solid; and taking the obtained reddish brown solid out of a centrifugal tube, centrifugally washing the solid for a plurality of times by using deionized water, and drying the solid in vacuum at the temperature of 60 ℃ to obtain the reddish brown iron oxide nano-particles.
FIG. 1 shows Fe prepared in this example2O3The X-ray diffraction pattern of the spherical nano-particles shows that the product is a pure-phase iron oxide compound.
FIG. 2 is Fe2O3As can be seen from fig. 2, the synthesized iron oxide sample is spherical nanoparticles, and the yield of iron oxide particles is more than 90% of the total amount and the particle size is uniform according to the estimation of the observation result of the scanning electron microscope. FIG. 3 is a partial enlarged view of FIG. 2, showing that the synthesized spherical iron oxide particles have a particle size ranging from 180 nm to 250 nm.
FIG. 4 is Fe2O3High resolution transmission electron micrographs of the samples. The selected area electron diffraction pattern of the spherical edge of iron oxide is shown as A, and can be indicated as single crystal electron diffraction of iron oxide. Indicating that the iron oxide sample is a single crystal nanoparticle. As can be seen from B, the sample crystallized well with the interplanar spacing consistent with that of iron oxide (003).
FIG. 5 is Fe2O3Rate capability and charge ofEfficiency-specific capacity curve of discharge, Fe2O3Under the condition that the sample is respectively cycled for 10 times and then returned to 100 mA/g under different current densities, the cycling curve shows that Fe2O3The specific discharge capacity of the material in the first turn of 100 mA/g, 200 mA/g, 500 mA/g and 1000 mA/g is 908 mAh/g, 698 mAh/g, 579 mAh/g and 488 mAh/g respectively, and the specific discharge capacity when the material returns to 100 mA/g is 701 mAh/g. As can be seen from the first-turn specific discharge capacity data, Fe2O3Is better due to Fe2O3The nano-structure is beneficial to the extraction and the insertion of lithium ions, and the nano-Fe with smaller particle size2O3The material can provide more lithium storage sites. Compared with other preparation methods, the method has the advantages of low preparation cost, simple synthesis process, uniform product appearance and good dispersibility. The electrochemical test result shows that the capacity retention rate of the iron oxide nanometer negative electrode material can be maintained at a higher level and has good stability.
Example 2
Mixing Fe (NO)3)3KCl and LiCl are mixed according to the mass ratio of 2: 20: 8, and are ground by using an agate mortar to achieve the effect of uniform mixing; collecting the mixture in an alumina crucible, putting the alumina crucible into a muffle furnace, heating to 780 ℃ at the speed of 5 ℃/min, roasting for 4 hours, and naturally cooling; soaking the product after reaction in deionized water to remove salt, and performing suction filtration to obtain a reddish brown solid; and taking the obtained reddish brown solid out of a centrifugal tube, centrifugally washing the solid for a plurality of times by using deionized water, and drying the solid in vacuum at the temperature of 60 ℃ to obtain the spherical reddish brown iron oxide nanoparticles.
Fig. 6 is a scanning electron microscope photograph of the iron oxide spherical nanoparticles prepared in this example, and it can be seen that the synthesized iron oxide is spherical nanoparticles with good dispersibility and a diameter of 800 to 1000 nm.
Example 3
FeC is added2O4KCl and LiCl are mixed according to the mass ratio of 2: 50: 20, and are ground by using an agate mortar to achieve the effect of uniform mixing; collecting the mixture in an alumina crucible and then putting the alumina crucible into a muffleHeating to 540 deg.C at a rate of 5 deg.C/min, calcining for 4 hr, and naturally cooling; soaking the product after reaction in deionized water to remove salt, and performing suction filtration to obtain a reddish brown solid; and taking the obtained reddish brown solid out of a centrifugal tube, centrifugally washing the solid for a plurality of times by using deionized water, and drying the solid in vacuum at the temperature of 60 ℃ to obtain the spherical reddish brown iron oxide nanoparticles.
Example 4
FeCO is added3KCl and LiCl are mixed according to the mass ratio of 2: 75: 30, and are ground by using an agate mortar to achieve the effect of uniform mixing; collecting the mixture in an alumina crucible, putting the alumina crucible into a muffle furnace, heating to 600 ℃ at the speed of 5 ℃/min, roasting for 4 hours, and naturally cooling; soaking the product after reaction in deionized water to remove salt, and performing suction filtration to obtain a reddish brown solid; and taking the obtained reddish brown solid out of a centrifugal tube, centrifugally washing the solid for a plurality of times by using deionized water, and drying the solid in vacuum at the temperature of 60 ℃ to obtain the spherical reddish brown iron oxide nanoparticles.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. However, the above description is only an example of the present invention, the technical features of the present invention are not limited thereto, and any other embodiments that can be obtained by those skilled in the art without departing from the technical solution of the present invention should be covered by the claims of the present invention.

Claims (4)

1. A molten salt synthesis method of iron oxide single crystal nano spherical particles is characterized by comprising the following steps:
(1) mixing iron salt, KCl and LiCl according to the mass ratio of 2: 50 x: 20x, wherein x is more than 0.2 and less than 2.2;
(2) collecting the mixture in an alumina crucible, putting the alumina crucible into a muffle furnace, heating to 530-800 ℃ at the speed of 5 ℃/min for roasting, wherein the roasting time is 2-6 h, and naturally cooling;
(3) soaking the product after reaction in deionized water to remove salt, and performing suction filtration to obtain a reddish brown solid;
(4) and taking the obtained reddish brown solid out of a centrifugal tube, centrifugally washing the solid for a plurality of times by using deionized water, and drying the solid in vacuum to obtain the spherical ferric oxide nano-particles.
2. The molten salt method for synthesizing iron oxide single crystal nano-spherical particles according to claim 1, wherein in the step 1, the iron salt comprises one or more of ferric nitrate, ferrous acetate, ferrous oxalate, ferric oxalate and ferrous carbonate.
3. The molten salt method for synthesizing iron oxide single crystal nano spherical particles according to claim 1, wherein in the step 1, the uniform mixing process is performed by grinding and mixing with an agate mortar.
4. The molten salt synthesis method of iron oxide single crystal nano spherical particles according to claim 1, wherein in the step 4, the temperature for vacuum drying is 40 to 80 ℃.
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Citations (3)

* Cited by examiner, † Cited by third party
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CN103172124A (en) * 2013-04-17 2013-06-26 新疆大学 Method for preparing ferric oxide three-dimensional nanostructure through solid-state chemical reaction
CN109338466A (en) * 2018-09-02 2019-02-15 景德镇陶瓷大学 It is a kind of to prepare monocrystalline Fe2O3The method of nano-particles self assemble elliptical shape ball micro nano structure
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CN101037232A (en) * 2007-04-26 2007-09-19 安徽工业大学 Method for preparing radius-controllable ferric oxide hollow ball
US20090090886A1 (en) * 2007-10-09 2009-04-09 The Research Foundation Of State University New York. Single-crystalline hematite rhombohedra and magnetic nanocomposites of iron and magnetite and methods of making same
CN101468817B (en) * 2007-12-25 2010-12-08 中国科学院过程工程研究所 Mesoporous nanocrystalline assembled porous bengala microsphere and preparation thereof

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Publication number Priority date Publication date Assignee Title
CN103172124A (en) * 2013-04-17 2013-06-26 新疆大学 Method for preparing ferric oxide three-dimensional nanostructure through solid-state chemical reaction
CN109338466A (en) * 2018-09-02 2019-02-15 景德镇陶瓷大学 It is a kind of to prepare monocrystalline Fe2O3The method of nano-particles self assemble elliptical shape ball micro nano structure
CN110510676A (en) * 2019-08-12 2019-11-29 江苏理工学院 A kind of LiFeO2Nano particle and preparation method thereof

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