CN104229900A - Preparation method of alpha-Fe2O3 cubes - Google Patents

Preparation method of alpha-Fe2O3 cubes Download PDF

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CN104229900A
CN104229900A CN201410467136.3A CN201410467136A CN104229900A CN 104229900 A CN104229900 A CN 104229900A CN 201410467136 A CN201410467136 A CN 201410467136A CN 104229900 A CN104229900 A CN 104229900A
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preparation
cubes
fe2o3
alpha
urea
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CN104229900B (en
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马谦
杨萍
卢盼盼
车全德
王俊鹏
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University of Jinan
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University of Jinan
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Abstract

The invention discloses a preparation method of alpha-Fe2O3 cubes. The preparation method comprises the following steps: by taking an iron salt as an iron source and urea as a hydroxide ion initiator and adding the two materials to an alcohol solvent, and stirring so that the raw materials can be mixed evenly to obtain a precursor solution of a solvothermal reaction; heating the precursor solution to the range of 180-220 DEG C and preserving heat for reacting for 6-36 hours; centrifuging the product after cooling, washing the obtained deposition phase, and after washing, drying the obtained deposition phase to obtain the alpha-Fe2O3 cubes which are controllable in dimension and the edges of the cubes are 0.1-1.0 micron long. The preparation method of the alpha-Fe2O3 cubes has the advantages that the raw material cost is low, the preparation process is simple, the alpha-Fe2O3 cubes different in edge length can be obtained by changing the addition ratio and the concentrations of the iron salt and the urea, the reaction temperature and the heat preservation time, nucleation is easy to control in the reaction process, the yield of the product is high, and large-scale synthesis of the micron/nano-scale alpha-Fe2O3 cubes can be realized.

Description

A kind of α-Fe 2o 3the preparation method of cubic block
Technical field
The present invention relates to a kind of α-Fe of technical field of chemical engineering 2o 3the preparation method of cubic block, especially relates to the α-Fe that a kind of length of side is controlled 2o 3the preparation method of cubic block.
Background technology
Ferric oxide is the important transition metal oxide material of a class, there is the advantages such as nontoxicity, cheap, good stability, physical and chemical performance are good, range of application is very extensive, can be used as sensitive material, catalytic material, making optics and electron device, magnetic recording material etc., cause the research interest of people.And α-Fe 2o 3be the most stable phase of thermodynamics of ferric oxide, its energy gap is 2.1eV, has larger specific surface area, demonstrates excellent characteristic in catalysis, biological medicine engineering, air-sensitive etc.
In recent years, the α-Fe of various micro-nano-scale has been prepared by the liquid phase of different system or gas-phase synthesizing method 2o 3material, comprises micro-nano granules, micro-nano mitron, cubic block, bar-shaped, the special appearance such as plate-like, needle-like, dendroid.Wherein, both at home and abroad about the α-Fe of varying particle size 2o 3the report of cubic block is also few.Peng Sun, Chen Wang, the " α-Fe of Copper-cladding Aluminum Bar of Xin Zhou etc. 2o 3sheet cubes: synthesis and gas-sensitive property " (Cu-doped α-Fe 2o 3hierarchical microcubes:synthesis and gas sensing properties. Sensors and Actuators B:Chemical, 2014,193:616-622) with iron(ic) chloride, urotropin for raw material, as solvent after the mixing of second alcohol and water, solvent-thermal method is utilized to synthesize at 160 DEG C of insulation 12 h the α-Fe that the length of side is 1.2 μm 2o 3cubic block.Chunyang Yin, Manickam Minakshi, David E. Ralph etc. " take glycine as raw material, water heat transfer cubes α-Fe 2o 3particle: Surface Characterization, reaction mechanism and electrochemical activity " (Hydrothermal synthesis of cubic α-Fe 2o 3microparticles using glycine:surface characterization, reaction mechanism and electrochemical activity. 2011,509,9821-9825) with iron(ic) chloride, glycine for raw material, water, as solvent, utilizes hydrothermal method to synthesize the α-Fe of the length of side for 0.3-1.3 μm 160 DEG C of insulation for some time 2o 3cubic block.But in prior art, synthesis α-Fe 2o 3expensive raw material price and large mainly with water as solvent, size regulating effect is not good.
Present stage, usually adopt hydro-thermal or solvent-thermal process legal system for the α-Fe of different size 2o 3cubic block structure, due to the restriction of differential responses system, raw materials cost is higher, the productive rate of product is on the low side, size regulating effect is not good.Therefore, study the high and controlled effective preparation method of size of a kind of productive rate simple to operate, reproducible, low raw-material cost, product, seem particularly important.
Summary of the invention
The present invention is directed to the problems referred to above, provide the α-Fe that a kind of productive rate simple to operate, reproducible, low raw-material cost, product is high, can realize having different size dimension 2o 3the controlledly synthesis of cubic block.
Technical scheme of the present invention is:
A kind of α-Fe 2o 3the preparation method of cubic block, is characterized in that, comprises the following steps:
A. be source of iron with molysite, urea is hydroxide ion initiator, source of iron and urea are joined in alcohol, by stirring, raw material being mixed, obtaining the precursor liquid of solvent thermal reaction;
B. moved in reactor by above-mentioned precursor liquid, be heated to 180-220 DEG C, insulation 6-36 h carries out solvent thermal reaction;
C. by centrifugal after above-mentioned reacted product cooling, the sediment-filled phase of gained is washed, and after washing, drying obtains α-Fe 2o 3cubic block.
In described step a, molysite and urea mol ratio are 1:7-16, and the concentration of molysite in alcohol is 0.06-0.15 mol/L.
Molysite in described step a is iron halide or iron nitrate.
Alcohol in described step a is ethanol or propyl alcohol.
α-Fe in described step c 2o 3the length of side of cubic block is 0.1-1.0 μm.
The present invention prepares α-Fe by solvent-thermal method 2o 3cubic block tool has the following advantages:
1. the present invention is hydroxide ion initiator with urea in solvent thermal reaction process, adopt alcohol as solvent, avoid the use of toxic substance and cost is low, each raw material can be mixed uniformly without the need to carrying out other operations, simple to operate, using alcohol as solvent, the control to Product size better can be realized.
2. reproducible, low raw-material cost, product the productive rate of the present invention high, can accomplish scale production;
3. the present invention is by the concentration of the additional proportion and molysite that change molysite and urea, temperature of reaction and soaking time, can to α-Fe 2o 3cubic block size dimension controls, the α-Fe of synthesis 0.1-1.0 μm of mass-producing 2o 3cubic block.
Accompanying drawing explanation
Fig. 1 is α-Fe prepared by the embodiment of the present invention 2 2o 3scanning electron microscope (SEM) picture of cubic block.
Fig. 2 is α-Fe prepared by the embodiment of the present invention 3 2o 3scanning electron microscope (SEM) picture of cubic block.
Fig. 3 is α-Fe prepared by the embodiment of the present invention 4 2o 3x-ray diffraction (XRD) collection of illustrative plates of cubic block.
Fig. 4 is α-Fe prepared by the embodiment of the present invention 4 2o 3scanning electron microscope (SEM) picture of cubic block.
Fig. 5 is α-Fe prepared by the embodiment of the present invention 8 2o 3scanning electron microscope (SEM) picture of cubic block.
Fig. 6 is scanning electron microscope (SEM) picture of the sample of comparative example 1 of the present invention preparation.
Embodiment
Below by embodiment, the present invention will be further elaborated, and following explanation has been only explanation the present invention, do not limit its content.
embodiment 1
The urea of the Fe(NO3)39H2O of 1.010 g, 1.100 g joins in 17 mL propanol solvent by 1, stirs and obtains clear solution;
Above-mentioned solution is transferred in reactor by 2, reacts 10 h at 180 DEG C;
3 products are after centrifugation and washing, and drying obtains the α-Fe that the length of side is 0.14-0.19 μm 2o 3cubic block.
embodiment 2
The urea of the ferric chloride hexahydrate of 0.676 g, 1.200 g joins in 25 mL alcohol solvents by 1, stirs and obtains clear solution;
Above-mentioned solution is transferred in reactor by 2, reacts 16 h at 200 DEG C;
3 products are after centrifugation and washing, and drying obtains the α-Fe that the length of side is 0.31-0.44 μm 2o 3cubic block, as shown in Figure 1.
embodiment 3
The urea of the ferric chloride hexahydrate of 0.676 g, 1.800 g joins in 25 mL alcohol solvents by 1, stirs and obtains clear solution;
Above-mentioned solution is transferred in reactor by 2, reacts 16 h at 200 DEG C;
3 products are after centrifugation and washing, and drying obtains the α-Fe that the length of side is 0.45-0.53 μm 2o 3cubic block, as shown in Figure 2.
embodiment 4
The urea of the ferric chloride hexahydrate of 0.676 g, 1.500 g joins in 25 mL alcohol solvents by 1, stirs and obtains clear solution;
Above-mentioned solution is transferred in reactor by 2, reacts 16 h at 200 DEG C;
3 products are after centrifugation and washing, and drying obtains α-Fe 2o 3cubic block.Respectively as shown in Figures 3 and 4, result shows α-Fe for the microscopic appearance of product and phase structure 2o 3the length of side of cubic block is 0.48-0.70 μm, and X-ray diffraction peak value and JCPDS card (33-0664) are consistent, and product is α-Fe 2o 3phase.
embodiment 5
The urea of the ferric chloride hexahydrate of 0.676 g, 1.650 g joins in 35 mL propanol solvent by 1, stirs and obtains clear solution;
Above-mentioned solution is transferred in reactor by 2, reacts 33 h at 190 DEG C;
3 products are after centrifugation and washing, and drying obtains the α-Fe that the length of side is 0.67-0.75 μm 2o 3cubic block.
embodiment 6
The urea of the Fe(NO3)39H2O of 1.010 g, 1.400 g joins in 40 mL propanol solvent by 1, stirs and obtains clear solution;
Above-mentioned solution is transferred in reactor by 2, reacts 30 h at 220 DEG C;
3 products are after centrifugation and washing, and drying obtains the α-Fe that the length of side is 0.87-0.95 μm 2o 3cubic block.
embodiment 7
The urea of the Fe(NO3)39H2O of 1.010 g, 2.000 g joins in 18 mL alcohol solvents by 1, stirs and obtains clear solution;
Above-mentioned solution is transferred in reactor by 2, reacts 7 h at 200 DEG C;
3 products are after centrifugation and washing, and drying obtains the α-Fe that the length of side is 0.52-0.64 μm 2o 3cubic block.
embodiment 8
The urea of the ferric chloride hexahydrate of 0.676 g, 2.100 g joins in 25 mL alcohol solvents by 1, stirs and obtains clear solution;
Above-mentioned solution is transferred in reactor by 2, reacts 16 h at 200 DEG C;
3 products are after centrifugation and washing, and drying obtains the α-Fe that the length of side is 0.40-0.48 μm 2o 3cubic block, as shown in Figure 5.
embodiment 9
The urea of the Fe(NO3)39H2O of 1.010 g, 2.390 g joins in 28 mL propanol solvent by 1, stirs and obtains clear solution;
Above-mentioned solution is transferred in reactor by 2, reacts 23 h at 180 DEG C;
3 products are after centrifugation and washing, and drying obtains the α-Fe that the length of side is 0.52-0.61 μm 2o 3cubic block.
comparative example 1
The urea of the ferric chloride hexahydrate of 0.676 g, 0.900 g joins in 25 mL alcohol solvents by 1, stirs and obtains clear solution;
Above-mentioned solution is transferred in reactor by 2, reacts 16 h at 200 DEG C;
3 products are after centrifugation and washing, and drying obtains the hollow microsphere structure that diameter is 2.2-2.8 μm, and as shown in Figure 6, its structural unit mostly is Ellipsoid shaped particle.
comparative example 2
The urea of the Fe(NO3)39H2O of 1.010 g, 3.050 g joins in 20 mL propanol solvent by 1, stirs and obtains clear solution;
Above-mentioned solution is transferred in reactor by 2, reacts 4 h at 180 DEG C;
3 products are after centrifugation and washing, and drying obtains product, and the sample of synthesis is irregular particle, and without special appearance, particle size distribution range is large.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not by the restriction of embodiment; other is any do not deviate from spirit of the present invention and principle under make change, modification, combination, substitute, simplify and all should be equivalent substitute mode, be included within protection scope of the present invention.

Claims (5)

1. a α-Fe 2o 3the preparation method of cubic block, is characterized in that, comprises the following steps:
A. be source of iron with molysite, urea is hydroxide ion initiator, source of iron and urea are joined in alcohol, by stirring, raw material being mixed, obtaining the precursor liquid of solvent thermal reaction;
B. moved in reactor by above-mentioned precursor liquid, be heated to 180-220 DEG C, insulation 6-36 h carries out solvent thermal reaction;
C. by centrifugal after above-mentioned reacted product cooling, the sediment-filled phase of gained is washed, and after washing, drying obtains α-Fe 2o 3cubic block.
2. preparation method according to claim 1, is characterized in that: in step a, molysite and urea mol ratio are 1:7-16, and the concentration of molysite in alcohol is 0.06-0.15 mol/L.
3. preparation method according to claim 1, is characterized in that: the molysite in step a is iron halide or iron nitrate.
4. preparation method according to claim 1, is characterized in that: the alcohol in step a is ethanol or propyl alcohol.
5. preparation method according to claim 1, is characterized in that: α-Fe in step c 2o 3the length of side of cubic block is 0.1-1.0 μm.
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106698522A (en) * 2016-09-13 2017-05-24 济南大学 Preparation method of alpha-Fe2O3 cube and microsphere
CN107265509A (en) * 2017-06-19 2017-10-20 华南理工大学 A kind of cubic nano-sized iron oxide and preparation method thereof
CN107356635A (en) * 2017-07-13 2017-11-17 济南大学 A kind of NiO nanometer sheets/α Fe applied to gas sensor2O3Nanocube heterojunction material
CN107698304A (en) * 2017-09-22 2018-02-16 芜湖新达园林绿化集团有限公司 One kind sustained release and good in economic efficiency epipremnum aureum dedicated fertilizer
CN107758748A (en) * 2017-11-28 2018-03-06 合肥学院 A kind of polyhedron di-iron trioxide and preparation method thereof
CN112408494A (en) * 2020-11-27 2021-02-26 台州学院 Preparation method of small-size ferric oxide cube
CN112897593A (en) * 2020-11-04 2021-06-04 河南海宏科技有限公司 Regular polyhedral alpha-Fe2O3Method for preparing self-growing material

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101041470A (en) * 2007-03-23 2007-09-26 清华大学 Method for synthesizing block-shaped alpha-ferric oxide nanostructure

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101041470A (en) * 2007-03-23 2007-09-26 清华大学 Method for synthesizing block-shaped alpha-ferric oxide nanostructure

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
XIAOQI FU等: "Surface-enhanced Raman scattering of 4-mercaptopyridine on sub-monolayers of α-Fe2O3 nanocrystals (sphere, spindle, cube)", 《J. RAMAN SPECTROSC.》 *

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106698522A (en) * 2016-09-13 2017-05-24 济南大学 Preparation method of alpha-Fe2O3 cube and microsphere
CN106698522B (en) * 2016-09-13 2018-03-30 济南大学 A kind of α Fe2O3The preparation method of cubic block and micron ball
CN107265509A (en) * 2017-06-19 2017-10-20 华南理工大学 A kind of cubic nano-sized iron oxide and preparation method thereof
CN107356635A (en) * 2017-07-13 2017-11-17 济南大学 A kind of NiO nanometer sheets/α Fe applied to gas sensor2O3Nanocube heterojunction material
CN107698304A (en) * 2017-09-22 2018-02-16 芜湖新达园林绿化集团有限公司 One kind sustained release and good in economic efficiency epipremnum aureum dedicated fertilizer
CN107758748A (en) * 2017-11-28 2018-03-06 合肥学院 A kind of polyhedron di-iron trioxide and preparation method thereof
CN112897593A (en) * 2020-11-04 2021-06-04 河南海宏科技有限公司 Regular polyhedral alpha-Fe2O3Method for preparing self-growing material
CN112897593B (en) * 2020-11-04 2023-03-10 河南海宏科技有限公司 Regular polyhedral alpha-Fe 2 O 3 Method for preparing self-growing material
CN112408494A (en) * 2020-11-27 2021-02-26 台州学院 Preparation method of small-size ferric oxide cube

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