Method for regulating and controlling oxygen defects of cerium dioxide nano material by pulse laser irradiation in liquid phase

A technology of pulsed laser and cerium oxide, which is applied in the fields of cerium oxide/cerium hydroxide, chemical instruments and methods, rare earth metal oxides/hydroxides, etc., can solve problems such as unfavorable, high energy consumption and high risk, and achieve Mild conditions, improved catalytic performance, and pure product

Active Publication Date: 2020-04-14
合肥中科纳普新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 energ...

Method used

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  • Method for regulating and controlling oxygen defects of cerium dioxide nano material by pulse laser irradiation in liquid phase
  • Method for regulating and controlling oxygen defects of cerium dioxide nano material by pulse laser irradiation in liquid phase
  • Method for regulating and controlling oxygen defects of cerium dioxide nano material by pulse 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 oxygen defects of a cerium dioxide nano material by pulse laser irradiation in a liquid phase, and the method comprises the following steps: dispersing CeO2 nanosheet powder in a solvent to prepare a 1mg/mL turbid liquid; wherein the solvent is at least one of water, methanol, ethanol or acetone; while stirring the turbid liquid, irradiating the turbid liquid for 5-60 minutes by adopting pulse laser with the wavelength of 355 nm or 532 nm, the pulse frequency of 20 Hz and the monopulse energy of 10-120 mJ; carrying out centrifugaltreatment, cleaning precipitates obtained by the centrifugal treatment by adopting deionized water, and then carrying out freeze drying to obtain the cerium dioxide nano material with reduced oxygendefects. The method is simple, safe, mild in condition, efficient and rapid in regulation and control process and environmentally friendly, other impurities are not introduced, and the pure and high-performance CeO2-x nano material with reduced oxygen defects can be obtained.

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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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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