CN113666382A - Preparation method of nano rare earth hexaboride - Google Patents

Preparation method of nano rare earth hexaboride Download PDF

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CN113666382A
CN113666382A CN202111065111.7A CN202111065111A CN113666382A CN 113666382 A CN113666382 A CN 113666382A CN 202111065111 A CN202111065111 A CN 202111065111A CN 113666382 A CN113666382 A CN 113666382A
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rare earth
hexaboride
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陈伟凡
刘正
彭荣
陈龙
叶剑勇
王立中
谢仁桂
梁海兵
邱振兴
蒋绪川
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Jiangxi Shanna New Material Technology Co Ltd
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    • C—CHEMISTRY; METALLURGY
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    • C01B35/02—Boron; Borides
    • C01B35/04—Metal borides
    • B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract

A process for preparing nano rare-earth hexaboride features that its chemical composition general formula is REB6The preparation method is mainly characterized in that: (1) according to REB6Weighing one or more of rare earth nitrate, rare earth oxide, sodium hydroxide rare earth or rare earth carbonate, mixing with nitric acid to prepare a rare earth nitrate solution, concentrating and evaporating; (2) weighing soluble chloride and adding the soluble chloride into the rare earth nitrate solution in the step (1); (3) weighing the organic fuel into the mixed solution in the step (2); (4) according to REB6Adding boron powder according to a stoichiometric ratio, uniformly stirring, and heating the mixed solution to concentrate to be in a viscous state. Then heating to initiate self-propagating combustion to obtain the product. The product is washed to obtain the nanometer rare earth hexaboride powder with stable structure. The method has the characteristics of simple process equipment, controllable particle size, no need of reducing atmosphere, quick reaction and easy industrialization.

Description

Preparation method of nano rare earth hexaboride
Technical Field
The invention belongs to the technical field of rare earth hexaboride preparation, and particularly relates to a preparation method of nano rare earth hexaboride.
Background
China is a big country of rare earth resources, and as an important cathode material, rare earth hexaboride (REB)6) Have been studied experimentally and theoretically for a long time. At REB6The cage structure combines the special 4f orbit of rare earth element and the electron deficiency characteristic of boron element, so that the material has many excellent properties of low work function, high conductivity, high emission current density, high hardness, high melting point, high chemical stability, strong heat radiation resistance and the like. Stefan S discovered nano LaB in 20036The infrared absorption coefficient in the near-infrared high energy density region (around 1000 nm) and the very high visible light transmittance (Journal of Applied Physics.2005 (97) (12),124314-124314 (8)). LaB6The consumption of the nano particles required for reaching the same shading coefficient is only one thirty times of the consumption of other materials, so the nano LaB6Can be widely applied to the fields of energy-saving glass, laser welding and the like. However, the large-scale controlled synthesis technology of nano lanthanum hexaboride is a bottleneck which restricts the wide application of nano lanthanum hexaboride.
So far, the preparation method of the nano rare earth hexaboride powder is always a hot point of research. For example, Chinese patent CN201010502217.4 discloses a rare earth hexaboride nano superfine powderThe preparation method comprises the steps of reacting a metal source raw material and a boron source raw material in the presence of a reducing agent in a reactor at 500-650 ℃ for 6-10 hours to obtain a rare earth boride product with the average particle size of 60-190 nm; chinese patent CN200610053497.9 reports that a synthetic method of nano hexaboride is obtained by preparing and preserving heat for 3-10 hours at 500-600 ℃ by using a high-pressure reaction kettle; chinese patent CN201010178836.2 describes a method for synthesizing metal boride nano-powder by iodine-assisted magnesium coreduction solid-phase reaction, wherein a certain pressure exists in a reaction system, and other reported hydrothermal method reaction conditions have the defects of harsh environmental requirements, complex equipment, high cost and the like.
Figure BDA0003258091410000011
D et al, which use active metals to prepare nano lanthanum hexaboride, require a long reaction time of at least 2 hours (Ceramics International.2012,38,8, 6203-. Von Silent CeO2、B2O3And Mg powder as raw material, KClO3As a heat generating agent, CeB is prepared6The micron powder is actually synthesized by reduction of active metal, and the obtained micron-sized rare earth hexaboride particles with the particle diameter of 0.64-1 μm (university of Lanzhou Ringchang, academic thesis, 2015.) are subjected to long-term shearing and crushing by a ball milling medium so as to change the micron particles into nanometer sizes by Takeda H and other people. The method has long synthesis period, takes at least 3 hours, The ball milling time is closely related to The size of primary particles, The time for reducing The ball milling time from 1 micron to 100nm needs to be longer than The synthesis period of micron particles, and The lanthanum hexaboride has high hardness, so that The ball milling medium is seriously abraded and The product is seriously polluted (Journal of The American Ceramic Society 2008,91(9): 2897) 2902). Kanakala R et al synthesizes LaB by solid phase combustion method6And Sm0.8B6The method for synthesizing the powder has the characteristics of simplicity, rapidness and energy conservation. The rare earth nitrate and carbohydrazide are ground and uniformly mixed and then ignited, so that hexaboride rare earth particles can be directly obtained, but the particle size can only be controlled to be about 500nmThe method has the problems that (1) carbohydrazide is carcinogenic and has high toxicity; (2) in the presence of nitric acid, the nitric acid is converted into a highly explosive compound carbonyl azide, so that the safety coefficient is low; (3) the solid-phase raw materials are mixed unevenly and take longer time; (4) rare earth nitrate is easy to absorb moisture and is not easy to accurately weigh. (Journal of the American Ceramic society.2010,93(10) 3136-3141.).
In summary, the existing synthesis method generally has the problems of poor performance of the prepared powder or high requirements on preparation equipment, atmosphere protection, long production period, difficulty in controlling conditions, high risk coefficient and the like. Aiming at the problems, the invention provides a chloride auxiliary solution combustion method for preparing nano rare earth hexaboride, soluble chloride is added into a solution combustion reaction mixture, so that the intensity of a combustion reaction can be reduced, the combustion process can be safely and controllably, the chloride can be precipitated in situ on the surface of product particles, the effective control of microstructures such as the size, the shape, the dispersity and the like of the product particles is realized, and the nano rare earth hexaboride is obtained.
Disclosure of Invention
Aiming at the technical bottleneck of the existing preparation of the nano rare earth hexaboride, the invention provides a simple, safe and quick preparation method of the nano rare earth hexaboride, which has a controllable structure, is green and does not need to control atmosphere.
A process for preparing nano rare-earth hexaboride features that the general chemical composition of nano rare-earth hexaboride is REB6Wherein RE is rare earth element, RE is one or more of La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb and Dy, and mainly comprises the following steps:
(1) according to REB6Weighing one or more of corresponding rare earth nitrate, rare earth oxide, rare earth hydroxide or rare earth carbonate according to the preparation amount and the stoichiometric ratio thereof to prepare a rare earth nitrate solution (1);
(2) weighing soluble chloride NaCl, KCl, LiCl or CaCl2Adding one or more of the rare earth nitrate solutions obtained in the step (1), and heating and dissolving to obtain a mixed solution (2);
(3) weighing one or more organic fuels of ethylene glycol, glycine, urea or citric acid, adding into the mixed solution (2), and heating for dissolving to obtain a mixed solution (3);
(4) according to REB6Weighing proper amount of boron powder according to the preparation amount and the stoichiometric ratio, uniformly stirring, and heating and concentrating to be viscous;
(5) heating the viscous liquid obtained in the step (4) to 200-350 ℃, initiating self-propagating combustion, finishing calcination, and taking out a combustion product;
(6) and (5) washing the combustion product obtained in the step (5) with dilute hydrochloric acid, dilute sulfuric acid and pure water in sequence, and drying to obtain the hexaboride rare earth nano powder.
In the step (2), the mole number of the chloride added is 0.1-3 times of that of the raw material rare earth ions.
The mole number of the organic fuel added in the step (3) is 0.1-5 times of that of the raw material rare earth ions.
The particle size of the boron powder added in the step (4) is less than 10 microns.
The invention has the characteristics of simple preparation process, low equipment requirement, no need of reducing atmosphere, quick reaction, controllable product particle size and easy industrialization.
Drawings
FIG. 1 is an X-ray diffraction spectrum of a sample of comparative example 1, which is shown in FIG. 1, compared with JCPDF #34-0427 card, and the sample is lanthanum hexaboride.
FIG. 2 is a scanning electron micrograph of the sample of comparative example 1, and as shown in FIG. 2, the particle size of the sample is about 500 nm.
FIG. 3 is an X-ray diffraction pattern of the sample of comparative example 2, which is shown in FIG. 3, comparing JCPDF #34-0427 card, the sample is lanthanum hexaboride.
FIG. 4 is a scanning electron micrograph of the sample of comparative example 2, and as shown in FIG. 4, the particle size of the sample is about 1 μm.
FIG. 5 is the X-ray diffraction pattern of the sample of example 1, as shown in FIG. 5, comparing JCPDF #34-0427 card, the sample is lanthanum hexaboride.
FIG. 6 is a SEM photograph of a sample of example 1, and as shown in FIG. 6, the particle size of the sample is mostly about 100 nm. Compared with the scanning electron micrographs of the samples of comparative examples 1 and 2, the particle size of the samples is obviously reduced, and the nano-scale powder is obtained.
FIG. 7 is an X-ray diffraction pattern of the sample of example 2, as shown in FIG. 7, comparing JCPDF #38-1455 card, the sample is cerium hexaboride.
FIG. 8 is a scanning electron micrograph of cerium hexaboride in example 2, and as shown in FIG. 8, the particle size of the sample is mostly about 100 nm.
FIG. 9 is the X-ray diffraction pattern of the synthesized sample of example 3, and comparing JCPDF #11-0087 card with that of FIG. 9, the sample is neodymium hexaboride.
FIG. 10 is a scanning electron micrograph of neodymium hexaboride in example 3, and as shown in FIG. 10, the particle size of the sample is mostly about 100 nm.
FIG. 11 is an X-ray diffraction pattern of the sample of example 4, as shown in FIG. 11, comparing JCPDF #36-1326 card, the sample is samarium hexaboride.
FIG. 12 is a scanning electron micrograph of samarium hexaboride in example 4, and as shown in FIG. 12, the particle size of the sample is mostly around 100 nm.
FIG. 13 is an X-ray diffraction pattern of the sample of example 5, as shown in FIG. 13, compared to JCPDF #40-1308 card, which was judged to be europium hexaboride.
FIG. 14 is a SEM photograph of a sample of example 5, and as shown in FIG. 14, the sample particle size is mostly around 100 nm.
Detailed Description
The present invention will be further illustrated by the following comparative examples and examples.
Comparative example 1
Respectively weighing 10.625g of lanthanum nitrate hexahydrate, 1.84g of glycine and 1.592g of boron powder in sequence, fully grinding and mixing in a mortar, then loading into a corundum crucible, placing into a muffle furnace, heating to 320 ℃, igniting reactants, taking out products after combustion is finished, washing with dilute hydrochloric acid, dilute sulfuric acid and pure water in sequence, and drying to obtain the sample.
Comparative example 2
10.635g of lanthanum nitrate hexahydrate and 1.84g of glycine were weighed out. Mix in a quartz beaker and add an appropriate amount of water to dissolve it completely. Then 1.592g of boron powder is added, the mixture is stirred evenly, heated and concentrated to be sticky, the mixture is put into a muffle furnace, and the temperature is raised to 320 ℃ to ignite the reactant. After the combustion is finished, taking out the product, washing the product by using dilute hydrochloric acid, dilute sulfuric acid and pure water in sequence, and drying the product to obtain a sample
Example 1
1.629g of lanthanum oxide is weighed, a proper amount of nitric acid is added into a quartz beaker to be heated and dissolved to prepare a lanthanum nitrate solution, 0.584g of sodium chloride and 0.75g of glycine are sequentially added to be heated and completely dissolved, 0.649g of boron powder is added to be uniformly stirred, the mixture is heated and concentrated to be viscous, the mixture is put into a muffle furnace, the temperature is increased to 320 ℃, reactants are ignited, products are taken out after combustion is finished, diluted hydrochloric acid, diluted sulfuric acid and pure water are sequentially used for washing, and the sample is obtained after drying.
Example 2
2.751g of cerium carbonate pentahydrate is weighed, and a proper amount of nitric acid is added into a quartz beaker to be heated and dissolved to prepare a cerium nitrate solution. Adding 0.584g of sodium chloride and 0.75g of glycine in sequence, heating to completely dissolve the sodium chloride and the glycine, adding 0.649g of boron powder, stirring uniformly, heating to concentrate the boron powder into a viscous state, putting the boron powder into a muffle furnace, heating to 320 ℃, and igniting the reactant. And after the combustion is finished, taking out the product, washing the product by using dilute hydrochloric acid, dilute sulfuric acid and pure water in sequence, and drying to obtain the sample.
Example 3
1.682g of neodymium oxide is weighed, and a proper amount of nitric acid is added into a quartz beaker to be heated and dissolved, so as to prepare a neodymium nitrate solution. Sequentially adding 1.168g of sodium chloride and 0.75g of glycine, heating to completely dissolve the sodium chloride and the glycine, adding 0.649g of boron powder, uniformly stirring, heating and concentrating to be viscous, putting into a muffle furnace, and heating to 300 ℃ for ignition. And after the combustion is finished, taking out the product, and then carrying out acid washing, water washing and drying on the product to obtain black powder.
Example 4
1.744g of samarium oxide is weighed, and a proper amount of nitric acid is added into a quartz beaker to be heated and dissolved to prepare samarium nitrate solution. 2.233g of potassium chloride and 0.75g of glycine are sequentially added, heated to be completely dissolved, then 0.649g of boron powder is added, stirred uniformly, heated and concentrated to be viscous, put into a muffle furnace, heated to 300 ℃ and ignited. And after the combustion is finished, taking out the product, washing the product by using dilute hydrochloric acid, dilute sulfuric acid and pure water in sequence, and drying to obtain the sample.
Example 5
1.76g of europium oxide is weighed, and a proper amount of nitric acid is added into a quartz beaker to be heated and dissolved to prepare europium nitrate solution. Sequentially adding 2.22g of calcium chloride and 0.75g of glycine, heating to completely dissolve, adding 0.649g of boron powder, uniformly stirring, heating and concentrating to be viscous, putting into a muffle furnace, heating to 290 ℃ and igniting. And after the combustion is finished, taking out the product, washing the product by using dilute hydrochloric acid, dilute sulfuric acid and pure water in sequence, and drying to obtain the sample.

Claims (4)

1. A method for preparing nano rare earth hexaboride is characterized by comprising the following steps: the chemical composition general formula of the nano rare earth hexaboride is REB6Wherein RE is rare earth element, RE is one or more of La, Ce, Pr, Nd, Pm, Sm, Eu, Gd, Tb and Dy, and mainly comprises the following steps:
(1) according to REB6Weighing one or more of rare earth nitrate, rare earth oxide, rare earth hydroxide or rare earth carbonate in proper amount according to the preparation amount and the stoichiometric ratio thereof to prepare rare earth nitrate solution (1);
(2) weighing soluble chloride NaCl, KCl, LiC or CaCl2Adding one or more of the rare earth nitrate solutions obtained in the step (1), and heating and dissolving to obtain a mixed solution (2);
(3) weighing one or more organic fuels of ethylene glycol, glycine, urea or citric acid, adding into the mixed solution (2), and heating for dissolving to obtain a mixed solution (3);
(4) according to REB6Weighing proper amount of boron powder according to the preparation amount and the stoichiometric ratio, uniformly stirring, and heating and concentrating to be viscous;
(5) heating the viscous liquid obtained in the step (4) to 200-350 ℃, initiating self-propagating combustion, finishing calcination, and taking out a combustion product;
(6) and (5) washing the combustion product obtained in the step (5) with dilute hydrochloric acid, dilute sulfuric acid and pure water in sequence, and drying to obtain the hexaboride rare earth nano powder.
2. The method for preparing nano rare earth hexaboride according to claim 1, wherein the mole number of chloride added in the step (2) is 0.1 to 3 times of that of the raw material rare earth ions.
3. The method for preparing nano rare earth hexaboride according to claim 1, wherein the mole number of the organic fuel added in the step (3) is 0.1 to 5 times of the mole number of the raw material rare earth ions.
4. The method for preparing nano rare earth hexaboride according to claim 1, wherein the particle size of the boron powder added in the step (4) is less than 10 μm.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110872122A (en) * 2019-12-04 2020-03-10 成都理工大学 NbB6Process for preparing nanoparticles
CN114956109A (en) * 2022-06-09 2022-08-30 陕西科技大学 Ultrahigh-temperature rare earth hexaboride powder and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5176890A (en) * 1987-11-26 1993-01-05 Rhone-Poulenc Chimie Preparation of rare earth borides
US20120177556A1 (en) * 2008-05-23 2012-07-12 Nevada, Reno Combustion synthesis method and boron-containing materials produced therefrom
CN103496730A (en) * 2013-10-12 2014-01-08 包头稀土研究院 Smelting process for producing rare earth oxide by recycling nitric acid and water
CN103524128A (en) * 2013-10-12 2014-01-22 南昌大学 Preparation method of yttria-stabilized zirconia tetragonal nano powder with high specific surface area

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5176890A (en) * 1987-11-26 1993-01-05 Rhone-Poulenc Chimie Preparation of rare earth borides
US20120177556A1 (en) * 2008-05-23 2012-07-12 Nevada, Reno Combustion synthesis method and boron-containing materials produced therefrom
CN103496730A (en) * 2013-10-12 2014-01-08 包头稀土研究院 Smelting process for producing rare earth oxide by recycling nitric acid and water
CN103524128A (en) * 2013-10-12 2014-01-22 南昌大学 Preparation method of yttria-stabilized zirconia tetragonal nano powder with high specific surface area

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110872122A (en) * 2019-12-04 2020-03-10 成都理工大学 NbB6Process for preparing nanoparticles
CN114956109A (en) * 2022-06-09 2022-08-30 陕西科技大学 Ultrahigh-temperature rare earth hexaboride powder and preparation method thereof

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