CN103232073B - Preparation method for nanometer iron oxide with correspondence matrix crystal boundaries - Google Patents

Preparation method for nanometer iron oxide with correspondence matrix crystal boundaries Download PDF

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CN103232073B
CN103232073B CN201310178107.0A CN201310178107A CN103232073B CN 103232073 B CN103232073 B CN 103232073B CN 201310178107 A CN201310178107 A CN 201310178107A CN 103232073 B CN103232073 B CN 103232073B
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iron plate
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alpha
crystal
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CN103232073A (en
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王乙潜
王超
梁文双
李春艳
蔡鎔声
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Qingdao University
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Abstract

The invention belongs to the technical field of nanometer materials and relates to a preparation method for nanometer iron oxide with correspondence matrix crystal boundaries. The preparation method comprises the steps of: firstly processing the surface of the high-purity iron sheet which is taken as an iron source by utilizing a sand blasting technique, then carrying out thermal oxidation reaction at 650 DEG C, and preparing petal-shaped nanometer alpha-Fe203 with the correspondence matrix crystal boundaries, wherein two sets of alpha-Fe203[0001] shaft-provided diffraction points can be used in an electronic diffraction pattern of the petal-shaped nanometer alpha-Fe203, each set of alpha-Fe203[0001] shaft-provided diffraction point represents a layer of crystals, the two sets of diffraction points can coincide by rotating, the rotation degrees are 27.80 degrees, sigma values of the crystal boundaries among the crystals are 13, and the alpha-Fe203 consists of an upper layer of single crystals and a lower layer of single crystals which are completely same. According to the preparation method, the preparation process is simple, the principle is reliable, the cost is low, the pollution is avoided, the material structure is novel, the performance is excellent, and the application range is wide.

Description

A kind of nano-sized iron oxide preparation method with coincidence lattice grain boundary
Technical field:
The invention belongs to technical field of nano material, relate to petal shaped nano ferric oxide (α-Fe that a kind of thermal oxidative reaction preparation has coincidence lattice grain boundary 2o 3) a kind of method, particularly nano-sized iron oxide preparation method with coincidence lattice grain boundary of twin crystal, its material of preparing can be used as sensor material, magnetic recording material and fine chemical material etc.
Background technology:
Under typical temperature, α-Fe 2o 3it in ferriferous oxide, is the most stable a kind of compound.α-Fe 2o 3be a kind of typical semiconductor material, band gap is 2.1eV, has the advantages such as cheapness, abundant raw material, environmental friendliness and high corrosion resistance.Due to quantum confined effect, surface effects and small-size effect, nanometer α-Fe 2o 3the physical and chemical performance that has many uniquenesses.Nanometer α-Fe 2o 3electricity lead temperature, humidity etc. more responsively, be a kind of sensor material that has development potentiality.In addition, due to nanometer α-Fe 2o 3there is good hardness and magnetic, thereby can be used as magneticsubstance and magnetic pipe recording material; Nanometer α-Fe 2o 3also there is good photostabilization, weathering resistance and chemical stability, so be again a kind of important mineral dye and fine chemical material.In a word, nanometer α-Fe 2o 3at aspects such as sensor, magneticsubstance and chemical industry, have a wide range of applications and be worth and DEVELOPMENT PROSPECT.In recent years, nanometer α-Fe 2o 3synthetic and property research be a study hotspot of field of nanometer material technology.At present, existing much about nanometer α-Fe 2o 3the achievement in research report of pattern and the controlled preparation of size, for example, utilizes the methods such as electrochemical synthesis, hydrothermal method, solvent-thermal method to prepare the nanometer α-Fe of the different morphologies such as particulate state, wire, sheet 2o 3.But these methods can only be to nanometer α-Fe 2o 3surface topography and size control, cannot well control its inner microtexture, as crystal boundary, defect etc.The microtexture of material has extremely important impact to the physical and chemical performance of material, and especially coincidence lattice grain boundary structure can significantly improve mechanical property, electric property and the magnetic performance of material, and therefore preparation has the nanometer α-Fe of coincidence lattice grain boundary 2o 3there is important practical usage.Adopt thermal oxidation method the at high temperature oxidizing reaction preparation of highly purified iron plate to be there is to the petal shaped nano α-Fe of coincidence lattice grain boundary 2o 3technique means not yet have at present report.
Summary of the invention:
The object of the invention is to overcome the shortcoming that prior art exists, seeking design provides a kind of thermal oxidative reaction that utilizes on high purity iron plate, to prepare the petal shaped nano α-Fe with coincidence lattice grain boundary 2o 3method, prepared nanometer α-Fe 2o 3because it has special coincidence lattice grain boundary, and there is excellent physical and chemical performance.
In order to realize foregoing invention object, the inventive method be take high purity iron plate as source of iron, first adopts sandblast technology to process iron plate surface, increases its surfaceness, then under 650 ° of C, carry out thermal oxidative reaction, make the petal shaped nano α-Fe with coincidence lattice grain boundary 2o 3, its concrete steps comprise:
(1) first adopt commercial blast technology, selecting diameter is the quartz sand of 180-220 μ m, to purity, be 99.99%, length is 5cm, and width is 3cm, and thickness is that sandblasting is carried out on the iron plate surface of 300 μ m, the sandblast time is 10s, pressure is 0.6MPa, the iron plate surface irregularity after gained is processed, and surfaceness is 1.8-3 μ m;
(2) with deionized water, the iron plate surface after to sandblasting is rinsed, and removes the impurity such as quartz sand and iron filings, then the iron plate after rinsing is placed in ultrasonic cleaner with ethanol ultrasonic cleaning 5min, obtains the iron plate after cleaning;
(3) by the iron plate after cleaning at N 2under environment, carry out conventional drying, remove its lip-deep impurity, obtain dried iron plate;
(4) more dried iron plate is put into conventional tube furnace, pass into purity and be 99.999% oxygen, regulate oxygen pressure to 35kPa, and be heated to 650 ° of C and carry out oxidizing reaction, temperature rise rate is 15 ° of C/min, and oxidization time is 1.5h;
(5) make to maintain in tube furnace oxygen and press constantly, iron plate is slowly down to room temperature, rate of temperature fall is 10 ° of C/min, obtains having the nanometer α-Fe of coincidence lattice grain boundary 2o 3; This α-Fe 2o 3selected area electron diffraction, in diffractogram can with two cover α-Fe 2o 3tape spool point diffraction, every cover point diffraction represents one deck α-Fe 2o 3crystal, two cover point diffractions can overlap by rotation, and angle of rotation α is 27.80 °; Theoretical according to coincidence site lattice, pivot 27.80 °, between resulting crystal, crystal boundary is that Σ value is 13 coincidence lattice grain boundary, prepared petal-shaped α-Fe 2o 3upper and lower two-layer identical single crystal, consist of, the torsion(al)angle between two-layer crystal is 27.80 °.
Compared with prior art, its product preparation process is simple for the inventive method, and principle is reliable, and production cost is low, pollution-free, prepared nanometer α-Fe 2o 3novel structure, excellent performance, applied range.
Accompanying drawing explanation:
Fig. 1 is the scanning electron microscope (SEM) photograph of the product prepared of the present invention, and wherein (a) is scanning electron microscope vertical view, is (b) scanning electron microscope sectional view.
Fig. 2 is the X-ray diffractogram of the product prepared of the present invention.
Fig. 3 is the transmission electron microscope results schematic diagram of the product prepared of the present invention, and wherein (a) is single α-Fe 2o 3transmission electron microscope bright field image, (b) be single α-Fe 2o 3selected area electron diffraction figure.
Embodiment:
Below by specific embodiment, also by reference to the accompanying drawings the inventive method is further elaborated.
Embodiment:
The present embodiment is implemented according to following concrete steps:
(1) first adopt commercial blast technology, selecting diameter is the quartz sand of 180-220 μ m, to purity, be 99.99%, length is 5cm, and width is 3cm, and thickness is that sandblasting is carried out on the iron plate surface of 300 μ m, the sandblast time is 10s, pressure is 0.6MPa, the iron plate surface irregularity after gained is processed, and surfaceness is 1.8-3 μ m;
(2) with deionized water, the iron plate surface after to sandblasting is rinsed, and removes the impurity such as quartz sand, iron filings, then the iron plate after rinsing is placed on to ethanol ultrasonic cleaning 5min in ultrasonic cleaner, obtains the iron plate after cleaning;
(3) by the iron plate after cleaning at N 2under environment, carry out conventional drying, remove its lip-deep impurity, obtain dried iron plate;
(4) more dried iron plate is put into tube furnace, pass into purity and be 99.999% oxygen, regulate oxygen pressure to 35kPa, and be heated to 650 ° of C and carry out oxidizing reaction, temperature rise rate is 15 ° of C/min, and oxidization time is 1.5h;
(5) in tube furnace, maintain oxygen and press constantly, iron plate is slowly down to room temperature, rate of temperature fall is 10 ° of C/min, obtains having the nanometer α-Fe of coincidence lattice grain boundary 2o 3;
Nano oxidized iron product prepared by the present embodiment is through the test analysis of various modern technologies, and its result has reached goal of the invention effect.The scanning electron microscope vertical view that Fig. 1 (a) is product, as can be seen from the figure grows petal-shaped structure on iron plate, and has larger density; The scanning electron microscope sectional view that Fig. 1 (b) is products obtained therefrom, can find out petal-shaped structure more clearly.Fig. 2 is the X-ray diffractogram of product, by contrast standard card, this diffractogram just can with α-Fe 2o 3match, so petal-like product is α-Fe 2o 3; Fig. 3 (a) is single α-Fe 2o 3transmission electron microscope bright field image, the contrast difference at edge can prove this α-Fe 2o 3there is twin crystal laminated structure; Fig. 3 (b) is this α-Fe 2o 3selected area electron diffraction, in diffractogram can with two cover α-Fe 2o 3tape spool point diffraction, every cover point diffraction represents one deck α-Fe 2o 3crystal, two cover point diffractions can overlap by rotation, and angle of rotation α is 27.80 °; Theoretical according to coincidence site lattice, pivot 27.80 °, between resulting crystal, crystal boundary is that Σ value is 13 coincidence lattice grain boundary, prepared petal-shaped α-Fe 2o 3upper and lower two-layer identical single crystal, consist of, the torsion(al)angle between two-layer crystal is 27.80 °.

Claims (1)

1. a nano-sized iron oxide preparation method with coincidence lattice grain boundary, is characterized in that: concrete steps comprise:
(1) first adopt commercial blast technology, selecting diameter is the quartz sand of 180-220 μ m, to purity, be 99.99%, length is 5cm, and width is 3cm, and thickness is that sandblasting is carried out on the iron plate surface of 300 μ m, the sandblast time is 10s, pressure is 0.6MPa, the iron plate surface irregularity after gained is processed, and surfaceness is 1.8-3 μ m;
(2) with deionized water, the iron plate surface after to sandblasting is rinsed, and removes quartz sand and iron filings impurity, then the iron plate after rinsing is placed in ultrasonic cleaner with ethanol ultrasonic cleaning 5min, obtains the iron plate after cleaning;
(3) by the iron plate after cleaning at N 2under environment, carry out conventional drying, remove its lip-deep impurity, obtain dried iron plate;
(4) more dried iron plate is put into conventional tube furnace, pass into purity and be 99.999% oxygen, regulate oxygen pressure to 35kPa, and be heated to 650 ° of C and carry out oxidizing reaction, temperature rise rate is 15 ° of C/min, and oxidization time is 1.5h;
(5) make to maintain in tube furnace oxygen and press constantly, iron plate is slowly down to room temperature, rate of temperature fall is 10 ° of C/min, obtains having the nanometer α-Fe of coincidence lattice grain boundary 2o 3; This α-Fe 2o 3selected area electron diffraction, in diffractogram with two cover α-Fe 2o 3tape spool point diffraction, every cover point diffraction represents one deck α-Fe 2o 3crystal, two cover point diffractions can overlap by rotation, theoretical according to coincidence site lattice, pivot 27.80 °, and between resulting crystal, crystal boundary is that Σ value is 13 coincidence lattice grain boundary, petal-shaped α-Fe 2o 3upper and lower two-layer identical single crystal, consist of, the torsion(al)angle between two-layer crystal is 27.80 °.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1364730A (en) * 2002-02-08 2002-08-21 无锡威孚吉大新材料应用开发有限公司 Method for preparing super-fine nanometer ferric oxide powder
CN1427042A (en) * 2001-12-17 2003-07-02 暨南大学 Manufacturing method of nano iron oxide powder
CN201267960Y (en) * 2008-09-18 2009-07-08 宝山钢铁股份有限公司 Pneumatic abrasive blaster

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1427042A (en) * 2001-12-17 2003-07-02 暨南大学 Manufacturing method of nano iron oxide powder
CN1364730A (en) * 2002-02-08 2002-08-21 无锡威孚吉大新材料应用开发有限公司 Method for preparing super-fine nanometer ferric oxide powder
CN201267960Y (en) * 2008-09-18 2009-07-08 宝山钢铁股份有限公司 Pneumatic abrasive blaster

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
Formation of modulated structures in single-crystalline hexagonal a-Fe2O3 nanowires;R. S. Cai et al.;《J Nanopart Res》;20120801;第14卷;第1-11页 *
R. S. Cai et al..Formation of modulated structures in single-crystalline hexagonal a-Fe2O3 nanowires.《J Nanopart Res》.2012,第14卷第1-11页.

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