Method for one-step microwave low-temperature preparation of large-granularity rare earth oxide

A rare earth oxide and large particle size technology, applied in the direction of rare earth metal oxide/hydroxide, lanthanide oxide/hydroxide, cerium oxide/cerium hydroxide, etc., can solve the problem of high sintering temperature, long time consumption, Energy consumption and other issues, to achieve the effect of uniform temperature distribution, low energy consumption, and avoid time waste

Pending Publication Date: 2022-05-24
CHINA NORTHERN RARE EARTH (GROUP) HIGH TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to provide a one-step low-temperature microwave method for preparing large-grained rare earth oxides. Using a microwave reactor to sinter and decompose, one-step continuous temperature rise can be realized, and microwave sintering in a low-temperature zone until the decomposition is complete; thus overcoming the existing It has the disadvantages of staged heating and heat preservation in microwave heating technology, long time consumption, high sintering temperature, and energy consumption.

Method used

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  • Method for one-step microwave low-temperature preparation of large-granularity rare earth oxide
  • Method for one-step microwave low-temperature preparation of large-granularity rare earth oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Put the lanthanum carbonate into the microwave reaction furnace, set the end temperature of sintering and heat preservation at 450 °C, set the automatic adjustment function of the microwave reaction furnace to turn on the microwave radiation at a heating rate of 10 °C / min; after heating to 450 °C, keep the temperature for 1 hour. Naturally cooled to room temperature to obtain the product lanthanum oxide. Through analysis and detection, RE0=99.65%, D50=36μm.

[0048] like figure 1 Shown is the XRD pattern of the large particle size lanthanum oxide prepared in Example 1 of the present invention.

[0049] The spectrum shows high diffraction intensity, complete peak shape, clear peak position and high product purity.

Embodiment 2

[0051] Put the neodymium praseodymium carbonate into the microwave reaction furnace, set the end temperature of sintering and heat preservation at 700 °C, set the automatic adjustment function of the microwave reaction furnace to turn on the microwave radiation at a heating rate of 6 °C / min;

[0052] After the temperature was raised to 700°C, the temperature was maintained for 2 hours. Naturally cooled to room temperature to obtain the product neodymium praseodymium oxide. Through analysis and detection, REO=99.38%, D50=29μm.

[0053] like figure 2 Shown is the scanning electron microscope image of the large particle size neodymium praseodymium oxide prepared in Example 2 of the present invention.

[0054] It can be seen in the figure that the crystal structure of the large-sized neodymium praseodymium oxide is clear, and all of them are spherical crystals composed of regular flaky wafers, and the crystal sizes are uniform.

Embodiment 3

[0056] Put lanthanum cerium oxalate into the microwave reaction furnace, set the end temperature of sintering and heat preservation at 550 °C, set the automatic adjustment function of the microwave reaction furnace to turn on microwave radiation at a heating rate of 8 °C / min; after heating to 550 °C, keep it for 1 hour . Naturally cooled to room temperature to obtain the product lanthanum cerium oxide. Through analysis and detection, REO=99.72%, D50=31μm.

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Abstract

The invention discloses a one-step microwave low-temperature preparation method of large-granularity rare earth oxide, which comprises the following steps: putting rare earth salt into a microwave reaction furnace, setting sintering heat preservation final temperature, setting temperature rise rate, and starting microwave radiation; carrying out microwave heating at a heating rate of 5-15 DEG C / min to 400-700 DEG C, and carrying out sintering and heat preservation; and naturally cooling to room temperature to obtain the large-granularity rare earth oxide of which the rare earth grade is greater than 99%. The microwave reaction furnace is used for sintering and decomposing, one-step continuous heating can be realized, and microwave sintering is performed in a low-temperature area until complete decomposition is realized; therefore, the defects of staged heating and heat preservation, long time consumption, high sintering temperature, energy consumption and the like in the existing microwave heating technology are overcome.

Description

technical field [0001] The invention belongs to the technical field of rare earth oxide preparation, and particularly relates to a one-step microwave low-temperature preparation method for large particle size rare earth oxide. Background technique [0002] Rare earth oxides have outstanding performance in the synthesis of rare earth functional ceramics and optical functional materials. The preparation of rare earth oxides by microwave can form an excellent crystal structure. This rare earth oxide has no optical anisotropy and is used in the synthesis process of various ceramics, optical glasses or optical functional materials. For example, when preparing transparent ceramics, doping rare earths Transparency after oxide is better than Al 2 O 3 It still has a linear transmittance of 80% in the far-infrared region, so it has been used in high temperature measuring holes, infrared detection windows, infrared components, high temperature lenses and discharge lamps and other occ...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): C01F17/206C01F17/229C01F17/235C01F17/241
CPCC01F17/206C01F17/229C01F17/241C01F17/235C01P2002/72C01P2004/03C01P2004/61C01P2006/80Y02P20/10
Inventor李婷婷刘威崔建国桑晓云徐占宇张国光高媛张文斌张永华尹少华
OwnerCHINA NORTHERN RARE EARTH (GROUP) HIGH TECH CO LTD