CN102173769A - Preparation method of rare earth ortho-ferrite nanometer powder - Google Patents

Preparation method of rare earth ortho-ferrite nanometer powder Download PDF

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CN102173769A
CN102173769A CN 201110029119 CN201110029119A CN102173769A CN 102173769 A CN102173769 A CN 102173769A CN 201110029119 CN201110029119 CN 201110029119 CN 201110029119 A CN201110029119 A CN 201110029119A CN 102173769 A CN102173769 A CN 102173769A
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preparation
rare earth
nano
aqueous solution
rare
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武安华
申慧
徐家跃
侍敏丽
罗丽庆
储耀卿
葛增伟
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Shanghai Institute of Ceramics of CAS
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Shanghai Institute of Ceramics of CAS
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Abstract

The invention discloses a preparation method of rare earth ortho-ferrite nanometer powder. The preparation method is a sol-gel spontaneous combustion method particularly comprising the following steps of: preparing a rare earth metal nitrate or hydrochloride water solution, a ferric nitrate or ferric chloride water solution and a citric acid water solution; mixing the prepared rare earth metal nitrate or hydrochloride water solution, the ferric nitrate or ferric chloride water solution and the citric acid water solution, and heating and stirring to form a sol-gel precursor; placing the obtained sol-gel precursor into a heating furnace at 550-650 DEG C for spontaneous combustion synthesis; and calcining an obtained spontaneous combustion product at 600-800 DEG C for 2-4 hours. The sol-gel spontaneous combustion method has the advantages of low energy consumption, simple preparation process without special equipment, high operability and product purity, suitability for large-scale production, and the like.

Description

A kind of preparation method of rare earth orthoferrite nano-powder
Technical field
The present invention relates to a kind of rare earth orthoferrite (ReFeO 3) preparation method of nano-powder, specifically, relate to a kind of method of utilizing sol-gel spontaneous combustion legal system to be equipped with the rare earth orthoferrite nano-powder, belong to the nano powder preparation technical field.
Background technology
The nanotechnology that grows up along with nano material preparation and applied research development has become one of present dominant technology.Because small-size effect, surface effects, quantum size effect and macroscopical tunnel effect etc. of nanoparticle make them present the characteristic that conventional material does not possess at aspects such as magnetic, light, electricity, for exploitation high-performance novel material provides opportunity widely.As the important component part of nanotechnology, the preparation of nano-powder has constituted the basis of nanotechnology.Rare earth orthoferrite (ReFeO 3) be composite oxide material with perovskite structure, as YFeO 3, TmFeO 3Deng, because their ion and electronic defects, they show unique physics and chemical property.This compounds has unique crystalline structure, especially lattice defect structure and the performance that after mixing, forms, be employed maybe and can be used in solid fuel cell, solid electrolyte, magneticsubstance, transmitter, the heat material, environmental monitoring, the numerous areas such as redox catalyst of solid resistor and alternative precious metal, become chemistry, the research focus in field such as physics and material, this compounds has broad application prospects as a class critical function material in the research in nanotechnology field, studies it and synthesizes, structure and special purpose are to chemical industry, industry such as machinery and even national defence have practical significance.
ReFeO 3The various performances of sill are subjected to the influence of a lot of aspects, and wherein powder quality is exactly a wherein the most key aspect.Along with the develop rapidly of modern science and technology, miniaturization of devices, Highgrade integration have become an important development trend, and preparation also becomes an important need with the synthetic high quality nano-powder that meets demand for development.
Sol-gel spontaneous combustion method is to be accompanied by the preparation of high-temp combustion synthetic further investigation and ultrapure ultrafine ceramic oxide the nineties in 20th century and a kind of low-cost preparation that occurs and the technology of synthetic single oxide and complex oxide, it is meant that redox reaction takes place for organic salt colloidal sol or organic salt and metal nitrate in heat-processed, the burning that reaction is brought out produces a large amount of gases, can self-keep and synthesize the material synthesis technique of required products of combustion.Compare with other technologies, the principal feature of this technology is that process is simple, does not need complex apparatus, and it is low to consume energy, and product purity is high.But do not see so far and utilize sol-gel spontaneous combustion legal system to be equipped with the relevant report of rare earth orthoferrite nano-powder.
Summary of the invention
The purpose of this invention is to provide a kind of method of utilizing sol-gel spontaneous combustion legal system to be equipped with the rare earth orthoferrite nano-powder, to satisfy ReFeO 3The wide application demand of sill.
For achieving the above object, the technical solution used in the present invention is as follows:
The preparation method of rare earth orthoferrite nano-powder provided by the invention is a sol-gel spontaneous combustion method, comprises following concrete steps:
A) the preparation rare-earth metal nitrate or the hydrochloride aqueous solution;
B) preparation iron nitrate or ferric chloride in aqueous solution;
C) preparation aqueous citric acid solution;
D) rare earth metal nitrate aqueous solution, iron nitrate aqueous solution or rare earth metal salt acid salt aqueous solution, the ferric chloride in aqueous solution with above-mentioned preparation mixes with aqueous citric acid solution, and heating is also stirred, and makes to form the sol-gel presoma;
E) the sol-gel presoma that obtains is inserted to carry out spontaneous combustion in 550～650 ℃ the process furnace synthetic;
F) the spontaneous combustion product that obtains was calcined 2～4 hours down at 600～800 ℃, ground, promptly get described rare earth orthoferrite nano-powder.
The rare-earth metal nitrate in the step a) or the hydrochloride aqueous solution can preparation get in the deionized water by rare-earth metal nitrate or hydrochloride are dissolved in, and also can get by rare-earth oxide being dissolved in prepare in nitric acid or the aqueous hydrochloric acid.
The concentration of the rare-earth metal nitrate in the step a) or the hydrochloride aqueous solution is recommended as 0.5～1.5mol/L.
Iron nitrate in the step b) or ferric chloride in aqueous solution can preparation get in the deionized water by iron nitrate or iron(ic) chloride are dissolved in, and also can pass through Fe 2O 3Be dissolved in and prepare in nitric acid or the aqueous hydrochloric acid and get.
The iron nitrate in the step b) or the concentration of ferric chloride in aqueous solution are recommended as 0.5～1.5mol/L.
The concentration of the aqueous citric acid solution in the step c) is recommended as 0.5～5.0mol/L.
Rare earth ion in the step d) and Fe 3+Mol ratio be recommended as 1: 1, the mol ratio of nitrate ion in the solution or chlorion and citric acid is recommended as 1: (1～4).
The formation temperature of the sol-gel presoma in the step d) is recommended as 70～90 ℃.
Process furnace in the step e) is recommended as retort furnace or resistance furnace.
Described rare earth is yttrium or lanthanide series rare-earth elements.
Compared with prior art, the present invention has following beneficial effect:
1) combustion flame temperature is lower, and is swift in response, and burning is synthesized in several minutes and can be finished, and has the low advantage of energy consumption;
Produce a large amount of gases when 2) burning, the detrimental impurity volatilization in the burning building-up process in the raw material is overflowed, play the self-purification effect, can obtain high purity product;
3) preparation technology is simple, need not specific installation, can be handling strong, accomplish scale production easily.
Description of drawings
Fig. 1 is the YFeO that embodiment 1 makes 3The XRD diffracting spectrum of nano-powder.
Specific implementation method
The present invention is described in further detail and completely below in conjunction with embodiment, but do not limit content of the present invention.
Embodiment 1
A) preparation Y (NO 3) 3The aqueous solution: the Y that takes by weighing 0.03mol 2O 3, the volumetric molar concentration that is dissolved in 40ml is in the aqueous nitric acid of 4.5mol/L;
B) preparation iron nitrate aqueous solution: the Fe that takes by weighing 0.03mol 2O 3, the volumetric molar concentration that is dissolved in 40ml is in the aqueous nitric acid of 4.5mol/L;
C) preparation aqueous citric acid solution: take by weighing the citric acid of 0.36mol, be dissolved in the deionized water of 72ml;
D) with the Y (NO of above-mentioned preparation 3) 3The aqueous solution, iron nitrate aqueous solution mix with aqueous citric acid solution, are heated to 80 ℃, stir to make to form the sol-gel presoma;
E) the sol-gel presoma that obtains is inserted to carry out spontaneous combustion in the retort furnace that is preheating to 600 ℃ synthetic;
F) the spontaneous combustion product that obtains was calcined 3 hours down at 700 ℃, ground, promptly get YFeO 3Nano-powder.
Fig. 1 is the YFeO that present embodiment makes 3The XRD diffracting spectrum of nano-powder, as seen from Figure 1: the crystalline structure of prepared nano-powder is complete, is pure YFeO 3There are not other impurity phases in phase.
Can calculate by the Scherrer formula and to learn prepared YFeO 3The particle diameter of nano-powder is 50～100nm.
Embodiment 2
The difference of present embodiment and embodiment 1 only is step a):
A) preparation Y (NO 3) 3The aqueous solution: the Y (NO that takes by weighing 0.06mol 3) 36H 2O is dissolved in the deionized water of 40ml.
All the other contents are all with identical described in the embodiment 1.
The prepared YFeO of present embodiment 3The XRD diffraction result of nano-powder is described identical with embodiment 1.
Embodiment 3
The difference of present embodiment and embodiment 1 only is step b):
B) preparation iron nitrate aqueous solution: the Fe (NO that takes by weighing 0.06mol 3) 39H 2O is dissolved in the deionized water of 40ml.
All the other contents are all with identical described in the embodiment 1.
The prepared YFeO of present embodiment 3The XRD diffraction result of nano-powder is described identical with embodiment 1.
Embodiment 4
The difference of present embodiment and embodiment 1 is step a) and step b):
A) preparation Y (NO 3) 3The aqueous solution: the Y (NO that takes by weighing 0.06mol 3) 36H 2O is dissolved in the deionized water of 40ml;
B) preparation iron nitrate aqueous solution: the Fe (NO that takes by weighing 0.06mol 3) 39H 2O is dissolved in the deionized water of 40ml.
All the other contents are all with identical described in the embodiment 1.
The prepared YFeO of present embodiment 3The XRD diffraction result of nano-powder is described identical with embodiment 1.
Embodiment 5
The difference of present embodiment and embodiment 1 only is step c):
C) preparation aqueous citric acid solution: take by weighing the citric acid of 0.90mol, be dissolved in the deionized water of 180ml.
All the other contents are all with identical described in the embodiment 1.
The prepared YFeO of present embodiment 3The XRD diffraction result of nano-powder is described identical with embodiment 1.
Embodiment 6
The difference of present embodiment and embodiment 1 only is step c):
C) preparation aqueous citric acid solution: take by weighing the citric acid of 1.44mol, be dissolved in the deionized water of 288ml.
All the other contents are all with identical described in the embodiment 1.
The prepared YFeO of present embodiment 3The XRD diffraction result of nano-powder is described identical with embodiment 1.
Embodiment 7
The difference of present embodiment and embodiment 1 only is step f):
F) the spontaneous combustion product that obtains was calcined 4 hours down at 600 ℃.
All the other contents are all with identical described in the embodiment 1.
The prepared YFeO of present embodiment 3The XRD diffraction result of nano-powder is described identical with embodiment 1.
Embodiment 8
The difference of present embodiment and embodiment 1 only is step f):
F) the spontaneous combustion product that obtains was calcined 2 hours down at 800 ℃.
All the other contents are all with identical described in the embodiment 1.
The prepared YFeO of present embodiment 3The XRD diffraction result of nano-powder is described identical with embodiment 1.
Embodiment 9
A) preparation YCl 3The aqueous solution: the Y that takes by weighing 0.025mol 2O 3, the volumetric molar concentration that is dissolved in 100ml is in the aqueous hydrochloric acid of 1.5mol/L;
B) preparation FeCl 3The aqueous solution: the Fe that takes by weighing 0.025mol 2O 3, the volumetric molar concentration that is dissolved in 100ml is in the aqueous hydrochloric acid of 1.5mol/L;
C) preparation aqueous citric acid solution: take by weighing the citric acid of 0.3mol, be dissolved in the deionized water of 600ml;
D) with the YCl of above-mentioned preparation 3The aqueous solution, FeCl 3The aqueous solution mixes with aqueous citric acid solution, is heated to 80 ℃, stirs to make to form the sol-gel presoma;
E) the sol-gel presoma that obtains is inserted to carry out spontaneous combustion in the retort furnace that is preheating to 600 ℃ synthetic;
F) the spontaneous combustion product that obtains was calcined 3 hours down at 700 ℃, ground, promptly get YFeO 3Nano-powder.
The prepared YFeO of present embodiment 3The XRD diffraction result of nano-powder is described identical with embodiment 1.
Embodiment 10
The difference of present embodiment and embodiment 9 only is step a):
A) preparation YCl 3The aqueous solution: the YCl that takes by weighing 0.05mol 36H 2O is dissolved in the deionized water of 100ml.
All the other contents are all with identical described in the embodiment 9.
The prepared YFeO of present embodiment 3The XRD diffraction result of nano-powder is described identical with embodiment 1.
Embodiment 11
The difference of present embodiment and embodiment 9 only is step b):
B) preparation FeCl 3The aqueous solution: the FeCl that takes by weighing 0.05mol 36H 2O is dissolved in the deionized water of 100ml.
All the other contents are all with identical described in the embodiment 9.
The prepared YFeO of present embodiment 3The XRD diffraction result of nano-powder is described identical with embodiment 1.
Embodiment 12
The difference of present embodiment and embodiment 9 is step a) and step b):
A) preparation YCl 3The aqueous solution: the YCl that takes by weighing 0.05mol 36H 2O is dissolved in the deionized water of 100ml;
B) preparation FeCl 3The aqueous solution: the FeCl that takes by weighing 0.05mol 36H 2O is dissolved in the deionized water of 100ml.
All the other contents are all with identical described in the embodiment 9.
The prepared YFeO of present embodiment 3The XRD diffraction result of nano-powder is described identical with embodiment 1.
In addition, experiment also proves: the Y in the foregoing description 2O 3The oxide compound Re of lanthanide series rare-earth elements that can equimolar amount 2O 3Be equal to alternative; Y (NO in the foregoing description 3) 3Nitrate Re (the NO of lanthanide series rare-earth elements that can equimolar amount 3) 3Be equal to alternative; YCl in the foregoing description 3The hydrochloride ReCl of lanthanide series rare-earth elements that can equimolar amount 3Be equal to alternative.

Claims (10)

1. the preparation method of a rare earth orthoferrite nano-powder is characterized in that: be sol-gel spontaneous combustion method, comprise following concrete steps:
A) the preparation rare-earth metal nitrate or the hydrochloride aqueous solution;
B) preparation iron nitrate or ferric chloride in aqueous solution;
C) preparation aqueous citric acid solution;
D) rare earth metal nitrate aqueous solution, iron nitrate aqueous solution or rare earth metal salt acid salt aqueous solution, the ferric chloride in aqueous solution with above-mentioned preparation mixes with aqueous citric acid solution, and heating is also stirred, and makes to form the sol-gel presoma;
E) the sol-gel presoma that obtains is inserted to carry out spontaneous combustion in 550～650 ℃ the process furnace synthetic;
F) the spontaneous combustion product that obtains was calcined 2～4 hours down at 600～800 ℃, ground, promptly get described rare earth orthoferrite nano-powder.
2. the preparation method of rare earth orthoferrite nano-powder according to claim 1, it is characterized in that: the rare-earth metal nitrate in the step a) or the hydrochloride aqueous solution are that preparation get in the deionized water by rare-earth metal nitrate or hydrochloride are dissolved in, or get by rare-earth oxide being dissolved in prepare in nitric acid or the aqueous hydrochloric acid.
3. the preparation method of rare earth orthoferrite nano-powder according to claim 1 is characterized in that: the concentration of the rare-earth metal nitrate in the step a) or the hydrochloride aqueous solution is 0.5～1.5mol/L.
4. the preparation method of rare earth orthoferrite nano-powder according to claim 1 is characterized in that: iron nitrate in the step b) or ferric chloride in aqueous solution are that preparation get in the deionized water by iron nitrate or iron(ic) chloride are dissolved in, or pass through Fe 2O 3Be dissolved in and prepare in nitric acid or the aqueous hydrochloric acid and get.
5. the preparation method of rare earth orthoferrite nano-powder according to claim 1 is characterized in that: the iron nitrate in the step b) or the concentration of ferric chloride in aqueous solution are 0.5～1.5mol/L.
6. the preparation method of rare earth orthoferrite nano-powder according to claim 1 is characterized in that: the concentration of the aqueous citric acid solution in the step c) is 0.5～5.0mol/L.
7. the preparation method of rare earth orthoferrite nano-powder according to claim 1 is characterized in that: rare earth ion in the step d) and Fe 3+Mol ratio be 1: 1, the mol ratio of nitrate ion in the solution or chlorion and citric acid is 1: (1～4).
8. the preparation method of rare earth orthoferrite nano-powder according to claim 1 is characterized in that: the formation temperature of the sol-gel presoma in the step d) is 70～90 ℃.
9. the preparation method of rare earth orthoferrite nano-powder according to claim 1 is characterized in that: the process furnace in the step e) is retort furnace or resistance furnace.
10. according to the preparation method of each described rare earth orthoferrite nano-powder in the claim 1 to 9, it is characterized in that: described rare earth is yttrium or lanthanide series rare-earth elements.
CN 201110029119 2011-01-27 2011-01-27 Preparation method of rare earth ortho-ferrite nanometer powder Pending CN102173769A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102502868A (en) * 2011-09-30 2012-06-20 中海石油天野化工股份有限公司 Preparation method of La-Ce (rhodium-cerium) codoped gama-Fe2O3 nanomaterial
CN108484175A (en) * 2018-04-21 2018-09-04 董秀玲 A kind of conducting ceramic material and preparation method thereof
CN112390294A (en) * 2020-11-21 2021-02-23 江西善纳新材料科技有限公司 High near-infrared reflectivity rare earth pigment and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN1458118A (en) * 2003-04-24 2003-11-26 哈尔滨工程大学 Process for preparing nano permanent magnetic ferrite powder
CN1759456A (en) * 2003-03-25 2006-04-12 美蓓亚株式会社 Ferrite magnet and method for production thereof
CN101013622A (en) * 2005-12-19 2007-08-08 Tdk株式会社 Ferrite magnetic material

Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
CN1759456A (en) * 2003-03-25 2006-04-12 美蓓亚株式会社 Ferrite magnet and method for production thereof
CN1458118A (en) * 2003-04-24 2003-11-26 哈尔滨工程大学 Process for preparing nano permanent magnetic ferrite powder
CN101013622A (en) * 2005-12-19 2007-08-08 Tdk株式会社 Ferrite magnetic material

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102502868A (en) * 2011-09-30 2012-06-20 中海石油天野化工股份有限公司 Preparation method of La-Ce (rhodium-cerium) codoped gama-Fe2O3 nanomaterial
CN102502868B (en) * 2011-09-30 2014-04-30 中海石油天野化工股份有限公司 Preparation method of La-Ce (rhodium-cerium) codoped gama-Fe2O3 nanomaterial
CN108484175A (en) * 2018-04-21 2018-09-04 董秀玲 A kind of conducting ceramic material and preparation method thereof
CN108484175B (en) * 2018-04-21 2021-12-10 山东鹏程陶瓷新材料科技有限公司 Conductive ceramic material and preparation method thereof
CN112390294A (en) * 2020-11-21 2021-02-23 江西善纳新材料科技有限公司 High near-infrared reflectivity rare earth pigment and preparation method thereof

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Application publication date: 20110907