CN103232073A - 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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CN103232073A
CN103232073A CN2013101781070A CN201310178107A CN103232073A CN 103232073 A CN103232073 A CN 103232073A CN 2013101781070 A CN2013101781070 A CN 2013101781070A CN 201310178107 A CN201310178107 A CN 201310178107A CN 103232073 A CN103232073 A CN 103232073A
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iron plate
preparation
nanometer
alpha
crystal
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CN103232073B (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 heavy site battle array crystal 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 heavy site battle array crystal boundary 2O 3) method, particularly a kind of nano-sized iron oxide preparation method with heavy site battle array crystal boundary of twin crystal, the material of its preparation can be used as sensor material, magnetic recording material and fine chemical material etc.
Background technology:
Under typical temperature, α-Fe 2O 3It is the most stable a kind of compound in ferriferous oxide.α-Fe 2O 3Be a kind of typical semiconductor material, band gap is 2.1eV, has advantages such as cheapness, abundant raw material, environmental friendliness and high corrosion resistance.Since 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. relatively more responsively, be a kind of sensor material that development potentiality is arranged.In addition, because nanometer α-Fe 2O 3Have good hardness and magnetic, thereby can be used as magneticsubstance and magnetic pipe recording material; Nanometer α-Fe 2O 3Also have 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 3Value and DEVELOPMENT PROSPECT have a wide range of applications at aspects such as sensor, magneticsubstance and chemical industry.In recent years, nanometer α-Fe 2O 3Synthetic and property research be a research focus of field of nanometer material technology.At present, existing much about nanometer α-Fe 2O 3The achievement in research report of pattern and controllable size preparation for example, utilizes methods such as electrochemical synthesis method, hydrothermal method, solvent-thermal method to prepare the nanometer α-Fe of multiple patterns such as particulate state, wire, sheet 2O 3But these methods can only be to nanometer α-Fe 2O 3Surface topography and size control, can't its inner microtexture of better controlled, as crystal boundary, defective etc.The microtexture of material has extremely important influence to the physical and chemical performance of material, and especially heavy site battle array 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 heavy site battle array crystal boundary 2O 3Important practical usage is arranged.Adopt thermal oxidation method the oxidizing reaction preparation at high temperature of highly purified iron plate to be had the petal shaped nano α-Fe of heavy site battle array crystal boundary 2O 3Technique means report is not arranged at present as yet.
Summary of the invention:
The objective of the invention is to overcome the shortcoming that prior art exists, seeking to design provides a kind of thermal oxidative reaction that utilizes to prepare the petal shaped nano α-Fe with heavy site battle array crystal boundary at the high purity iron plate 2O 3Method, prepared nanometer α-Fe 2O 3Because it has special heavy site battle array crystal boundary, and excellent physical chemistry is arranged.
In order to realize the foregoing invention purpose, the inventive method is source of iron with the high purity iron plate, adopts sandblast technology to handle the iron plate surface earlier, increases its surfaceness, under 650 ° of C, carry out thermal oxidative reaction then, make the petal shaped nano α-Fe with heavy site battle array crystal boundary 2O 3, its concrete steps comprise:
(1) adopts the commercial blast technology earlier, selecting diameter for use is the quartz sand of 180-220 μ m, be 99.99% to purity, 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 handled, and surfaceness is 1.8-3 μ m;
(2) wash with the iron plate surface of deionized water after to sandblasting, remove impurity such as quartz sand and iron filings, the iron plate after will washing again is placed in the ultrasonic cleaner with ethanol ultrasonic cleaning 5min, the iron plate after obtaining to clean;
(3) iron plate after will cleaning is at N 2Carry out conventional drying under the environment, remove its lip-deep impurity, get dried iron plate;
(4) more dried iron plate is put into conventional tube furnace, fed 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 and keep oxygen in the tube furnace and press constantly, iron plate slowly is down to room temperature, rate of temperature fall is 10 ° of C/min, obtains having the nanometer α-Fe of heavy site battle array crystal boundary 2O 3This α-Fe 2O 3Selected area electron diffraction, in the diffractogram can with two the cover α-Fe 2O 3[0001] tape 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 °; According to heavy site battle array theory, around 27.80 ° of [0001] axle rotations, crystal boundary is that the Σ value is 13 heavy site battle array crystal boundary between resulting crystal, prepared petal-shaped α-Fe 2O 3Be made up of two-layer identical single crystal up and down, the torsion(al)angle between the two-layer crystal is 27.80 °.
The inventive method compared with prior art, its product preparation process is simple, principle is reliable, production cost is low, and is pollution-free, prepared nanometer α-Fe 2O 3Novel structure, excellent performance, applied range.
Description of drawings:
Fig. 1 is the sem photograph of the product of the present invention's preparation, and wherein (a) is the scanning electron microscope vertical view, (b) is the scanning electron microscope sectional view.
Fig. 2 is the X-ray diffractogram of the product of the present invention's preparation.
Fig. 3 is the transmission electron microscope results synoptic diagram of the product of the present invention's preparation, and wherein (a) is single α-Fe 2O 3The transmission electron microscope bright field image, (b) be single α-Fe 2O 3Selected area electron diffraction figure.
Embodiment:
Also by reference to the accompanying drawings the inventive method is further elaborated below by specific embodiment.
Embodiment:
Present embodiment is implemented according to following concrete steps:
(1) adopts the commercial blast technology earlier, selecting diameter for use is the quartz sand of 180-220 μ m, be 99.99% to purity, 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 handled, and surfaceness is 1.8-3 μ m;
(2) wash with the iron plate surface of deionized water after to sandblasting, remove impurity such as quartz sand, iron filings, the iron plate after will washing again is placed on ethanol ultrasonic cleaning 5min in the ultrasonic cleaner, the iron plate after obtaining to clean;
(3) iron plate after will cleaning is at N 2Carry out conventional drying under the environment, remove its lip-deep impurity, get dried iron plate;
(4) more dried iron plate is put into tube furnace, feed 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) keep oxygen in the tube furnace and press constantly, iron plate slowly is down to room temperature, rate of temperature fall is 10 ° of C/min, obtains having the nanometer α-Fe of heavy site battle array crystal boundary 2O 3
The nano oxidized iron product of present embodiment preparation is through the test analysis of various modern technologies, and its result has reached the goal of the invention effect.Fig. 1 (a) is the scanning electron microscope vertical view of product, as can be seen from the figure grows the petal-shaped structure on the iron plate, and bigger density is arranged; Fig. 1 (b) is the scanning electron microscope sectional view of products obtained therefrom, can find out the petal-shaped structure more clearly.Fig. 2 is the X-ray diffractogram of product, by the contrast standard card, this diffractogram just can with α-Fe 2O 3Be complementary, so petal-like product is α-Fe 2O 3Fig. 3 (a) is single α-Fe 2O 3The transmission electron microscope bright field image, the contrast difference at edge can prove this α-Fe 2O 3Has the twin crystal laminated structure; Fig. 3 (b) is this α-Fe 2O 3Selected area electron diffraction, in the diffractogram can with two the cover α-Fe 2O 3[0001] tape 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 °; According to heavy site battle array theory, around 27.80 ° of [0001] axle rotations, crystal boundary is that the Σ value is 13 heavy site battle array crystal boundary between resulting crystal, prepared petal-shaped α-Fe 2O 3Be made up of two-layer identical single crystal up and down, the torsion(al)angle between the two-layer crystal is 27.80 °.

Claims (1)

1. nano-sized iron oxide preparation method with heavy site battle array crystal boundary, it is characterized in that: concrete steps comprise:
(1) adopts the commercial blast technology earlier, selecting diameter for use is the quartz sand of 180-220 μ m, be 99.99% to purity, 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 handled, and surfaceness is 1.8-3 μ m;
(2) wash with the iron plate surface of deionized water after to sandblasting, remove quartz sand and iron filings impurity, the iron plate after will washing again is placed in the ultrasonic cleaner with ethanol ultrasonic cleaning 5min, the iron plate after obtaining to clean;
(3) iron plate after will cleaning is at N 2Carry out conventional drying under the environment, remove its lip-deep impurity, get dried iron plate;
(4) more dried iron plate is put into conventional tube furnace, fed 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 and keep oxygen in the tube furnace and press constantly, iron plate slowly is down to room temperature, rate of temperature fall is 10 ° of C/min, obtains having the nanometer α-Fe of heavy site battle array crystal boundary 2O 3This α-Fe 2O 3Selected area electron diffraction, in the diffractogram with two the cover α-Fe 2O 3[0001] tape spool point diffraction, every cover point diffraction represents one deck α-Fe 2O 3Crystal, two cover point diffractions can overlap by rotation, and according to heavy site battle array theory, around 27.80 ° of [0001] axle rotations, crystal boundary is that the Σ value is 13 heavy site battle array crystal boundary between resulting crystal, petal-shaped α-Fe 2O 3Be made up of two-layer identical single crystal up and down, the torsion(al)angle between the 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 (1)

* Cited by examiner, † Cited by third party
Title
R. S. CAI ET AL.: "Formation of modulated structures in single-crystalline hexagonal a-Fe2O3 nanowires", 《J NANOPART RES》 *

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