CN104176759A - Molten salt method for preparing cubic massive CeO2 nanometer material - Google Patents

Molten salt method for preparing cubic massive CeO2 nanometer material Download PDF

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Publication number
CN104176759A
CN104176759A CN201410361116.8A CN201410361116A CN104176759A CN 104176759 A CN104176759 A CN 104176759A CN 201410361116 A CN201410361116 A CN 201410361116A CN 104176759 A CN104176759 A CN 104176759A
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China
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molten salt
salt method
nano
nanometer material
ceo
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CN201410361116.8A
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CN104176759B (en
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邓积光
何胜男
戴洪兴
谢少华
杨黄根
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Beijing University of Technology
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Beijing University of Technology
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Abstract

The invention relates to a molten salt method for preparing a cubic massive CeO2 nanometer material, and belongs to the technical field of nanometer material preparation. The molten salt method comprises the following steps: firstly uniformly mixing NaNO3, NaF and CeCl3 which are weighed in proportion, and then transferring the mixture into a muffle furnace; increasing temperature from room temperature to 450-550 DEG C at the velocity of 1 DEG C/minute, preserving heat for 3 hours, and naturally cooling to room temperature; and carrying out dissolution, suction filtration, washing and drying to obtain the cubic massive CeO2 nanometer material. The molten salt method disclosed by the invention has the advantages of simple preparation process, high phase purity, controllability in product shape, high output and the like, and raw materials are low in cost and easily available.

Description

One is prepared a cube block CeO 2the melting salt method of nano material
Technical field
The present invention relates to one and prepare a cube block CeO 2the melting salt method of nano material, relates to specifically with NaNO 3with NaF be melting salt system preparation cube block CeO 2the melting salt method of nano material, belongs to field of nano material preparation.
Background technology
Rare earth is a kind of very important strategic resources, has very important effect in Chinese national economy construction, is often used to high-quality precision and sophisticated technology industry.In recent years, be accompanied by the development of nanotechnology, many traditional materials show the using value making new advances.For example, traditional rare earth material and nanotechnology are combined, prepare rare earth nano material, and explore its application at environmental catalysis chemical fields such as motor-vehicle tail-gas improvement and receive much attention.
Cerium oxide (CeO 2) as a kind of light rare earths oxide compound, there is purposes very widely.At present, CeO 2nearly ten thousand tons of year consumptions of powder, its application performance is not only relevant with purity and structure, and granularity, dispersiveness and pattern etc. are to CeO 2the application of powder also has larger impact.Therefore, the CeO of preparation high purity, polymolecularity and regular pattern 2nano particle is further broaden application field and the key that improves utilising efficiency.For the preparation of CeO 2the method of nano particle mainly comprises: the precipitator method, hydrothermal method, microemulsion method and sol-gel method etc.Owing to thering is higher surfactivity, in dry and roasting process, easily make CeO 2nanoparticle agglomerates or sintering, thus cause gained nano particle diameter to increase, weaken CeO 2the catalytic performance of nano particle.
Melting salt method is the novel method of the development in recent years preparation nano material of getting up.The method has that raw material is cheap and easy to get, preparation process is simple, cost is low, product purity is high and output advantages of higher.For example: (Hu little Ping, waits .CeO to Guo etc. for Guo Guibao, Wang Zhengde 2one step scorification preparation and characterization of nano-powder. rare earth, 2008,29 (6): 17-20) with NaNO 3/ LiNO 3for melting salt system, prepare CeO 2superfine powder.It is worthy of note, there is no at present at NaNO 3in/NaF melting salt system, prepare a cube block CeO 2the bibliographical information of nano material.
Summary of the invention
The object of the present invention is to provide one to prepare a cube block CeO 2the melting salt method of nano material, is characterized in that the NaNO weighing in proportion 3, NaF and CeCl 3after mixing, be transferred in retort furnace, rise to 450-550 DEG C with the speed of 1 DEG C/min from room temperature, and constant temperature insulation 3h, naturally cool to room temperature, after water dissolution fused salt, suction filtration, washing, being dried, obtain a cube block CeO 2nano material.NaNO 3with the mass ratio of NaF be 49:1, (NaNO 3+ NaF) and CeCl 3mass ratio be 30:1.
It is cheap and easy to get that the present invention has raw material, and preparation process is simple, and product particle morphology and crystalline structure are controlled, and output advantages of higher.Gained cube block CeO 2nano material has a good application prospect at aspects such as electrode materials, catalyzer, superconducting material, sensor, synthetic gas production, environmental monitorings.Utilize the technology such as X-ray diffractometer (XRD) and scanning electronic microscope (SEM) to characterize respectively crystal phase structure and the particle morphology of sample.
Brief description of the drawings
Fig. 1 is gained cube block CeO 2the XRD spectra of nano material, wherein curve (a), (b) are respectively embodiment 1, embodiment 2 XRD spectra after roasting under 450 DEG C and 550 DEG C of conditions.
Fig. 2 is gained cube block CeO 2the SEM photo of nano material, wherein (a), (b) are respectively embodiment 1, the embodiment 2 SEM photo after roasting under 450 DEG C and 550 DEG C of conditions.
Embodiment
For further understanding the present invention, elaborate with embodiment below, and provide accompanying drawing and describe cube block CeO that the present invention obtains 2nano material, but the present invention is not limited to following examples.
Embodiment 1: by 29.4g NaNO 3, 0.6g NaF and 1g CeCl 3ball milling 15min, is transferred in retort furnace after mixing, and rises to 450 DEG C with the temperature rise rate of 1 DEG C/min from room temperature, and insulation 3h, naturally cools to room temperature subsequently, after dissolving, suction filtration, washing, being dried, can obtain a cube block CeO 2nano material.
Embodiment 2: by 29.4g NaNO 3, 0.6g NaF and 1g CeCl 3ball milling 15min, is transferred in retort furnace after mixing, and rises to 550 DEG C with the temperature rise rate of 1 DEG C/min from room temperature, and insulation 3h, naturally cools to room temperature subsequently, after dissolving, suction filtration, washing, being dried, can obtain a cube block CeO 2nano material.
Preparation method's novelty of the present invention, raw material cheapness, preparation process is simple, and product particle morphology is controlled and output is higher.Gained cube block CeO 2nano material has potential using value in fields such as environmental catalysis.

Claims (2)

1. prepare a cube block CeO for one kind 2the melting salt method of nano material, is characterized in that the NaNO weighing in proportion 3, NaF and CeCl 3after mixing, be transferred in retort furnace, rise to 450-550 DEG C with the speed of 1 DEG C of min from room temperature, and constant temperature insulation 3h, naturally cool to room temperature, after water dissolution melting salt, suction filtration, washing, being dried, obtain a cube block CeO 2nano material.
2. by the method for claim 1, NaNO 3with the mass ratio of NaF be 49:1, (NaNO 3+ NaF) and CeCl 3mass ratio be 30:1.
CN201410361116.8A 2014-07-27 2014-07-27 One prepares a cube block CeO 2the molte-salt synthesis of nano material Expired - Fee Related CN104176759B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106010468A (en) * 2016-06-22 2016-10-12 黄毅 Low-melting-point mixed molten salt as heat transfer and storage medium
CN106540713A (en) * 2016-11-03 2017-03-29 北京工业大学 A kind of original position prepares the molte-salt synthesis of iron sesquioxide loading platinum nanocatalyst
CN113044873A (en) * 2021-04-16 2021-06-29 陕西科技大学 CeO for chemical mechanical polishing2Nanoparticles and method for preparing same

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102189489A (en) * 2010-03-12 2011-09-21 株式会社Lg化学 Method for recycling cerium oxide abrasive
CN102583495A (en) * 2012-02-23 2012-07-18 清华大学 Preparation method of rare earth metal ion doping cerium oxide nanometer material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102189489A (en) * 2010-03-12 2011-09-21 株式会社Lg化学 Method for recycling cerium oxide abrasive
CN102583495A (en) * 2012-02-23 2012-07-18 清华大学 Preparation method of rare earth metal ion doping cerium oxide nanometer material

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
F.BONDIOLI, ET AL.: "Nanosized CeO2 powders obtained by flux method", 《MATERIALS RESEARCH BULLETIN》 *
郭贵宝等: "CeO2纳米粉体的一步熔融法制备及表征", 《稀土》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106010468A (en) * 2016-06-22 2016-10-12 黄毅 Low-melting-point mixed molten salt as heat transfer and storage medium
CN106540713A (en) * 2016-11-03 2017-03-29 北京工业大学 A kind of original position prepares the molte-salt synthesis of iron sesquioxide loading platinum nanocatalyst
CN113044873A (en) * 2021-04-16 2021-06-29 陕西科技大学 CeO for chemical mechanical polishing2Nanoparticles and method for preparing same

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