CN105776348A - Simple preparation method for micron-order magnetic alpha-iron trioxide particles - Google Patents

Simple preparation method for micron-order magnetic alpha-iron trioxide particles Download PDF

Info

Publication number
CN105776348A
CN105776348A CN201610300123.6A CN201610300123A CN105776348A CN 105776348 A CN105776348 A CN 105776348A CN 201610300123 A CN201610300123 A CN 201610300123A CN 105776348 A CN105776348 A CN 105776348A
Authority
CN
China
Prior art keywords
preparation
iron
magnetic
order magnetic
muffle furnace
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610300123.6A
Other languages
Chinese (zh)
Inventor
王俊宏
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shaanxi University of Technology
Original Assignee
Shaanxi University of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shaanxi University of Technology filed Critical Shaanxi University of Technology
Priority to CN201610300123.6A priority Critical patent/CN105776348A/en
Publication of CN105776348A publication Critical patent/CN105776348A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/02Oxides; Hydroxides
    • C01G49/06Ferric oxide [Fe2O3]
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/80Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/42Magnetic properties

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Compounds Of Iron (AREA)

Abstract

The invention discloses a simple preparation method for micron-order magnetic alpha-iron trioxide particles, belonging to the technical field of preparation processes of inorganic materials. To satisfy a heavy demand of magnetic materials in technological development and industrialization process, according to the method disclosed by the invention, an organic iron-containing compound is taken as an iron source, the micron-order magnetic alpha-iron trioxide particles which are uniform in size diameter and high in magnetic intensity are prepared by a simple high-temperature pyrolysis method, so that the preparation procedure of the magnetic alpha-iron trioxide is greatly simplified and is easy for industrial production. The method disclosed by the invention is expected to be widely applied in numerous fields, such as energy and chemical industry, environment protection and biotechnology.

Description

A kind of simple and convenient process for preparing of micron order magnetic α-iron sesquioxide particle
Technical field
The invention belongs to technical field of preparation for inorganic material, open one prepares micron order magnetic α-iron sesquioxide particle Short-cut method.
Technical background
α-iron sesquioxide is a kind of n-type semiconductor, and visible ray shows the response of preferable Optical Electro-Chemistry, The aspects such as the process of heterogeneous catalysis, sunlight absorbing material, lithium ion battery, chemical sensor and Organic Pollutants in Wastewater All it is widely used.
At present, the preparation method of magnetic α-iron sesquioxide is more, has microemulsion method, hydro-thermal method, Hydrolyze method, colloidal sol-solidifying Glue method, chemical precipitation method, pyrolysismethod, Microwave-assisted synthesis method, Radiation Synthesis Method and solid phase method etc..In all these preparations In method, thermal decomposition method technique is the simplest, and more convenient operation, cost is relatively low, applies wider.Reinforcement very waits Fe (NO3)3·9H2O Alcoholic solution thermal decomposition, prepared finely dispersed Nano red α-Fe2O3Powder (reinforcement is strange, Li Li, Wang Ling, Wang Wei, Thermal decomposition process of preparing nano α-Fe2O3, Wuhan University Of Technology's journal, 2001,24 (3): 251-252);Ma Zhenye etc. with Fe2(SO4)3·5H2O is source of iron, prepares, by coprecipitation, the submicron alpha-Fe that specific surface area is higher2O3(Ma Zhenye, Li Feng Raw, bigger serface α-Fe2O3Preparation and catalytic performance research, solid-rocket technology, 2006,29 (4): 286-288); Patent also has several preparation α-Fe in addition2O3Method, a kind of is the water generated by co-precipitation with oxalic acid solution with ferrous ion Conjunction Ferrox. is precursor, then roasting, it is thus achieved that pore-size distribution is narrower, the nanometer α-Fe that specific surface area is higher2O3(Wang Qihua, Wang Dewei, Wang Tingmei, the preparation method of a kind of α-phase ferricoxide, CN 102649587 A);One is with FeCl3·6H2O For source of iron, by solvent thermal decomposition method, prepare α-Fe2O3Nanosphere (Guo Xiaohui, Zhang Ji, a kind of α-Fe2O3Preparation method, CN 103922421 A);Also having one is also with FeCl3·6H2O is source of iron, prepares a kind of micron order olive by hydrothermal synthesis method Olive globular α-Fe2O3Material (Wang Zhiguo, Li Zhijie, Lin Zhijie, a kind of micron order American football shape iron oxide material and preparation side thereof Method, CN 105129864 A).In a word, at α-Fe2O3In numerous preparation methoies of material, some complicated process of preparation, cost Height, some use materials are poisonous, harmful, and have produces pollutant etc., many defects in preparation process, hinders preparation method Extensive application.Therefore α-Fe is explored2O3The greenization of material preparation method, preparation technology simplification imperative.
Summary of the invention
It is an object of the invention to provide a kind of micron order magnetic α-Fe2O3Simple and convenient process for preparing, expand α-Fe2O3's Range of application.The organic iron containing compounds ground is put in Muffle furnace, by high-temperature roasting, lower the temperature, cool down after obtain granularity Uniform micron order magnetic α-iron sesquioxide particle.
The concrete operation method of the present invention includes following key step:
1) organic iron containing compounds is ground to certain particle size, puts into crucible, be then placed in Muffle furnace;
2) with certain programming rate under oxygen or air atmosphere by step 1) in Muffle furnace rise to 500-800 DEG C, Insulation 2-6h, then allows Muffle furnace naturally be down to room temperature;
3) by step 2) in crucible after cooling take out, obtain having micron order magnetic α-three oxidation two of uniform particle size Iron particle.
Organic iron containing compounds mentioned by the present invention can be the one in ferric citrate or ferric ammonium citrate.
Iron containing compounds sample granularity mentioned by the present invention is less than 100 mesh.
Programming rate mentioned by the present invention is 1-10 DEG C/min.
The major advantage of preparation method involved in the present invention: be that preparation technology is very simple, so can significantly contract Short preparation time.Through micron order magnetic α-Fe prepared by this method2O3Particle, even particle size distribution, mean diameter is 1.3 μm, Saturation magnetization is 19.52eum/g.
Accompanying drawing explanation
Magnetic α-the Fe of preparation in Fig. 1: embodiment 12O3The x-ray diffraction pattern of particle.
Magnetic α-the Fe of preparation in Fig. 2: embodiment 12O3The grain size distribution of particle.
Magnetic α-the Fe of preparation in Fig. 3: embodiment 12O3The hysteresis curve figure of particle.
Detailed description of the invention
Following embodiment is further illustrating rather than limiting the scope of the present invention of the present invention.
Embodiment 1
2g ferric ammonium citrate is put in mortar and grind, put into crucible, place in Muffle furnace, with 10 DEG C/min's Programming rate rises to 550 DEG C from room temperature under air conditions, is incubated 3h, then naturally cools to room temperature, obtain micron order magnetic α-Fe2O3Sample, its mean diameter is 1.3 μm, and saturation magnetization is 19.52emu/g.
From Fig. 1 it can be seen that preparation magnetic α-Fe2O3The X-ray diffraction of particle occurs in the range of 20-80 ° Diffraction maximum, respectively corresponding (012), (104), (110), (006), (113), (202), (024), (116), (018), (214), (300), (208), (1010), (220) and (036) peak, be α-Fe2O3Absworption peak, illustrate by this method The material of preparation is typical α-Fe2O3Magnetic material;From Fig. 2 it can be seen that preparation α-Fe2O3The particle diameter distribution of particle Narrower, mean diameter concentrates on about 1.3 μm;From Fig. 3 it can be seen that preparation α-Fe2O3The magnetic hysteresis loop tool of particle Having narrower Magnetic hysteresis ring, its saturation magnetization is 19.52emu/g.
Embodiment 2
2g ferric citrate granule is ground in mortar, puts into crucible, place in Muffle furnace, with 10 DEG C/min's Programming rate rises to 650 DEG C from room temperature under air conditions, is incubated 2h, then naturally cools to room temperature, obtain micron order magnetic α-Fe2O3Sample.
Embodiment 3
3g ferric ammonium citrate granule is ground in mortar, puts into crucible, place in Muffle furnace, with 5 DEG C/min's Programming rate rises to 600 DEG C from room temperature under air conditions, is incubated 4h, then naturally cools to room temperature, obtain micron order magnetic α-Fe2O3Sample.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, those skilled in the art can So that the raw material used in the present invention and proportioning are modified without departing from the spirit and scope of the present invention.So, if originally These variations of invention belong within the scope of the claims in the present invention and equivalent technologies thereof, then the present invention is also intended to comprise these and changes Including moving.

Claims (5)

1. the simple and convenient process for preparing of micron order magnetic α-iron sesquioxide particle, it is characterised in that:
The organic iron containing compounds ground is put in Muffle furnace, by high-temperature roasting, lower the temperature, cool down after obtain even-grained Micron order magnetic α-iron sesquioxide particle.
2. the preparation method as described in right 1 requires, it is characterised in that comprise the steps:
1) organic iron containing compounds is ground to certain particle size, puts into crucible, be then placed in Muffle furnace;
2) with certain programming rate, by step 1 under oxygen or air atmosphere) in Muffle furnace rise to 500-800 DEG C, protect Temperature 2-6h, then allows Muffle furnace naturally be down to room temperature;
3) by step 2) in cooling after crucible take out, obtain even-grained micron order magnetic α-iron sesquioxide particle.
3. the preparation method as described in right 1 or 2 requires, it is characterised in that above-mentioned mentioned organic iron containing compounds can be One in ferric citrate or ferric ammonium citrate.
4. the preparation method as described in right 1 or 2 requires, it is characterised in that above-mentioned mentioned iron containing compounds sample granularity is low In 100 mesh.
5. the preparation method as described in right 1 or 2 requires, it is characterised in that above-mentioned mentioned programming rate is 1-10 DEG C/min.
CN201610300123.6A 2016-05-03 2016-05-03 Simple preparation method for micron-order magnetic alpha-iron trioxide particles Pending CN105776348A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610300123.6A CN105776348A (en) 2016-05-03 2016-05-03 Simple preparation method for micron-order magnetic alpha-iron trioxide particles

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610300123.6A CN105776348A (en) 2016-05-03 2016-05-03 Simple preparation method for micron-order magnetic alpha-iron trioxide particles

Publications (1)

Publication Number Publication Date
CN105776348A true CN105776348A (en) 2016-07-20

Family

ID=56401008

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610300123.6A Pending CN105776348A (en) 2016-05-03 2016-05-03 Simple preparation method for micron-order magnetic alpha-iron trioxide particles

Country Status (1)

Country Link
CN (1) CN105776348A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107746081A (en) * 2017-11-10 2018-03-02 河南理工大学 A kind of preparation method of two-dimensional nano piece form α Fe2O3 materials
CN111499370A (en) * 2020-05-20 2020-08-07 中国科学院重庆绿色智能技术研究院 Preparation method of coated ferromagnetic material

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101898749B (en) * 2010-08-02 2014-07-02 武汉理工大学 Method for preparing metal oxide hollow particles or fibers

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101898749B (en) * 2010-08-02 2014-07-02 武汉理工大学 Method for preparing metal oxide hollow particles or fibers

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
严新: "固相法制备氧化铁纳米粒子", 《盐城工学院学报(自然科学版)》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107746081A (en) * 2017-11-10 2018-03-02 河南理工大学 A kind of preparation method of two-dimensional nano piece form α Fe2O3 materials
CN107746081B (en) * 2017-11-10 2019-06-18 河南理工大学 A kind of two-dimensional nano piece form α-Fe2O3The preparation method of material
CN111499370A (en) * 2020-05-20 2020-08-07 中国科学院重庆绿色智能技术研究院 Preparation method of coated ferromagnetic material

Similar Documents

Publication Publication Date Title
Silambarasu et al. Room-temperature superparamagnetism and enhanced photocatalytic activity of magnetically reusable spinel ZnFe 2 O 4 nanocatalysts
Vignesh et al. Photocatalytic activity of magnetically recoverable MnFe2O4/g-C3N4/TiO2 nanocomposite under simulated solar light irradiation
Zhang et al. Magnetic Fe3O4@ C/Cu and Fe3O4@ CuO core–shell composites constructed from MOF-based materials and their photocatalytic properties under visible light
Grasset et al. Synthesis and magnetic characterization of zinc ferrite nanoparticles with different environments: powder, colloidal solution, and zinc ferrite− silica core− shell nanoparticles
Liu et al. Synthesis and characteristics of Sm2O3 and Nd2O3 nanoparticles
Chinnaraj et al. Comparative studies of microwave-and sol-gel-assisted combustion methods of Fe 3 O 4 nanostructures: structural, morphological, optical, magnetic, and catalytic properties
Yang et al. Clean and reproducible SERS substrates for high sensitive detection by solid phase synthesis and fabrication of Ag‐coated Fe3O4 microspheres
Ismail et al. Synthesis and characterization of iron-doped TiO2 nanoparticles using ferrocene from flame spray pyrolysis
Wilson et al. Preparation and photocatalytic properties of hybrid core–shell reusable CoFe2O4–ZnO nanospheres
Chaiwichian et al. Highly efficient visible-light-induced photocatalytic activity of Bi2WO6/BiVO4 heterojunction photocatalysts
Singh et al. Newly developed Fe3O4–Cr2O3 magnetic nanocomposite for photocatalytic decomposition of 4-chlorophenol in water
Rameshbabu et al. Synthesis of superparamagnetic ZnFe 2 O 4 nanoparticle by surfactant assisted hydrothermal method
CN104495950A (en) Preparation method of carbon encapsulated magnetic C/Fe3O4 nano composite material and application thereof
Xu et al. Synthesis and performance of novel magnetically separable nanospheres of titanium dioxide photocatalyst with egg-like structure
CN103785426B (en) BiOCl base heterojunction of a kind of visible light catalysis activity and preparation method thereof
YV Synthesis and characterization of magnetically core-shell structured CoFe2O4/SiO2 nanoparticles; their enhanced antibacterial and electrocatalytic properties
Suresh et al. Fabrication of iron oxide nanoparticles: magnetic and electrochemical sensing property
CN106745305A (en) A kind of α Fe2O3The preparation method of magnetic nano powder material
CN105776348A (en) Simple preparation method for micron-order magnetic alpha-iron trioxide particles
Yang et al. The study on degradation and separation of RhB under UV light by magnetically ZnO/Fe2O3 nanoparticles
Cervera-Gabalda et al. Tuning the photocatalytic performance through magnetization in Co-Zn ferrite nanoparticles
CN106944030B (en) A kind of preparation and its application of oxygen sensitivity conductor oxidate nano material
Bhosale et al. Influence of morphology and crystallinity on field emission properties of NiFe2O4 nanoparticles grown by high-temperature vapor phase condensation route
CN103933993B (en) Photochemical catalyst nanometer Eu capable of magnetic separating 3+-CoFe 2o 4raw powder's production technology
Panda et al. Effect of Zn concentration on microstructural, optical, and hyperfine properties of nanocrystalline α-Fe 2 O 3

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20160720