A method for regulating oxygen vacancies in ceria nanomaterials by pulsed laser irradiation in liquid phase

A technology of pulsed lasers and nanomaterials, applied in cerium oxide/cerium hydroxide, chemical instruments and methods, lanthanide oxides/hydroxides, etc., can solve problems such as unfavorable, high energy consumption and high risk, and achieve The effect of mild conditions, improved catalytic performance, and efficient and rapid regulation process

Active Publication Date: 2022-02-01
合肥中科纳普新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The aforementioned regulation of CeO 2 The method of oxygen deficiency either uses high temperature conditions or uses explosive reducing gas, which has the disadvantages of high energy consumption and high risk, and inevitably introduces impurities and by-products, which is not conducive to the regulation of pure and high-performance ceria nanomaterials oxygen deficiency

Method used

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  • A method for regulating oxygen vacancies in ceria nanomaterials by pulsed laser irradiation in liquid phase
  • A method for regulating oxygen vacancies in ceria nanomaterials by pulsed laser irradiation in liquid phase
  • A method for regulating oxygen vacancies in ceria nanomaterials by pulsed laser irradiation in liquid phase

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Experimental program
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Embodiment approach

[0027] (1) The solvent is at least one of water, methanol, ethanol or acetone. By adding CeO 2 Nanosheet powder dispersed in different solvents and pulsed laser irradiation can prepare CeO with different sizes and concentrations of oxygen defects 2-x nanomaterials.

[0028] (2) In order to prevent CeO 2 Sedimentation occurs and it is ensured that it is uniformly irradiated by pulsed laser light. During the irradiation process, it is necessary to supplement the suspension with continuous magnetic stirring.

[0029] (3) The pulse laser is a nanosecond parallel pulse laser emitted by a Nd:YAG nanosecond pulse laser.

[0030] (4) By adjusting the laser parameters such as the wavelength, pulse frequency, single pulse energy, and irradiation time of the pulse laser, CeO with different sizes and different concentrations of oxygen defects can be prepared.2-x nanomaterials.

[0031] (5) Oxygen defects in the ceria nanomaterials prepared by the present invention mainly exist in the ...

Embodiment 1

[0036] A method for regulating oxygen defects in ceria nanomaterials by pulsed laser irradiation in a liquid phase, comprising the following steps:

[0037] Step 1, the CeO 2 The nanosheet powder was dispersed in methanol and prepared into 0.3mg / mL, 0.5mg / mL, 1mg / mL and 2mg / mL white suspensions respectively.

[0038] Step 2. Carry out magnetic stirring to the four kinds of suspensions respectively, the magnetic stirring speed is 500r / min, and while carrying out magnetic stirring to the suspension, use a wavelength of 355nm, a pulse width of 7ns, a pulse frequency of 20Hz, a single pulse Pulsed laser with an energy of 50mJ irradiated the four kinds of suspensions for 10 minutes respectively, and then centrifuged, and the precipitate obtained from the centrifuged treatment was repeatedly washed with deionized water for 3 to 4 times, and then freeze-dried to obtain yellow-green Ceria nanomaterials with reduced oxygen defects.

[0039] Specifically, at the same time, a portion o...

Embodiment 2

[0041] A method for regulating oxygen defects in ceria nanomaterials by pulsed laser irradiation in a liquid phase, comprising the following steps:

[0042] Step 1, the CeO 2 The nanosheet powder was dispersed in ethanol to prepare a 1 mg / mL white suspension.

[0043] Step 2. Magnetically stir the suspension with stirring speeds of 100r / min, 500r / min and 1500r / min respectively, and while magnetically stirring the suspension, use a wavelength of 355nm and a pulse width of 7ns, pulse frequency of 20Hz, single pulse energy of 50mJ pulsed laser irradiates the suspension, and it is easy to cause CeO 2 The precipitation of the sample makes the irradiation inhomogeneous, and it is easy to cause the suspension to splash out at a high stirring rate, so the optimal stirring rate in the embodiment of the present invention is 500r / min; The suspension was irradiated for 10 minutes, then centrifuged, and the precipitate obtained by the centrifuged treatment was repeatedly washed 3 to 4 ti...

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Abstract

The invention discloses a method for regulating and controlling the oxygen deficiency of ceria nanomaterials by pulsed laser irradiation in the liquid phase. CeO 2 The nanosheet powder is dispersed in a solvent and prepared into a suspension of 1 mg / mL; the solvent is at least one of water, methanol, ethanol or acetone; while the suspension is stirred, a wavelength of 355nm or 532nm, a pulse frequency of 20Hz, and a single pulse energy of 10-120mJ pulsed laser irradiate the suspension for 5-60 minutes, then perform centrifugation, and use deionized water to clean the precipitate obtained from the centrifugation, and then Freeze-drying is carried out to prepare ceria nanomaterials with reduced oxygen defects. The present invention is not only simple and safe, has mild conditions, efficient and fast regulation process, and is green and environmentally friendly, but also does not introduce other impurities, and can obtain CeO with pure, high performance and reduced oxygen defects. 2‑x nanomaterials.

Description

technical field [0001] The invention relates to the technical field of preparation of ceria nanomaterials, in particular to a method for regulating and controlling oxygen defects of ceria nanomaterials by pulsed laser irradiation in a liquid phase. Background technique [0002] CeO 2 It is an important rare earth oxide, which is widely used in catalysis, magnetism, optics, electrochemistry and other technical fields because of its special electronic structure and unique physical and chemical properties. The electronic structure of Ce is 4f 1 5d 1 6s 2 , the absence of 5d, 6s (three electrons) or 4f, 5d, 6s (four electrons) orbital electrons can occur, so CeO 2 The Ce atoms in the middle can form Ce 3+ and Ce 4+ The two valence states are stable and can occur depending on the treatment conditions (oxygen partial pressure and redox environment). 3+ and Ce 4+ The mutual transformation between, and then caused the CeO 2 The formation and disappearance of oxygen defects ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F17/235B01J23/10B01J37/34B82Y30/00
CPCB01J23/10B01J35/004B01J37/349B82Y30/00
Inventor 梁长浩吕佳丽田振飞叶一星刘俊
Owner 合肥中科纳普新材料有限公司
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