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ZrO2 with micro/nano structure and preparation method of ZrO2

A nanostructure and nanosphere technology, applied in the fields of nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., to achieve the effects of easy operation, cheap and easily available raw materials, and simple and novel methods

Inactive Publication Date: 2015-04-29
SHIJIAZHUANG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, for the hydrothermal synthesis of ZrO induced by biomolecules and complexed by EDTA molecules 2 research has not yet been reported

Method used

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  • ZrO2 with micro/nano structure and preparation method of ZrO2
  • ZrO2 with micro/nano structure and preparation method of ZrO2
  • ZrO2 with micro/nano structure and preparation method of ZrO2

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preparation example Construction

[0042] The present invention also discloses a kind of above-mentioned micro / nano structure ZrO 2 The preparation method comprises the following steps:

[0043] S1. The parts by weight are respectively 0.1-0.3 parts of β-cyclodextrin and 1.5-2.6 parts of ZrOCl 2 .8H 2 O, 1.9-2.2 parts of EDTA and 1.68 parts of NaHCO 3 Dissolve in 50 parts of water to obtain a mixed solution;

[0044] S2. Transfer the above-mentioned mixed solution system to a high-pressure reactor, and heat-treat at 150-220° C. for 5-30 hours;

[0045] S3. After the heat treatment, the autoclave is naturally cooled at room temperature, and then the precipitate is separated and washed with deionized water. After drying or calcination, the micro / nanostructure ZrO 2 .

[0046] In step S1, β-cyclodextrin, ZrOCl can be added to the water in sequence 2 .8H 2 O, EDTA and NaHCO 3 , to get a mixed solution after fully stirring; you can also add β-cyclodextrin and ZrOCl in water first 2 .8H 2 O, stir well befor...

Embodiment 1

[0049] The preparation method comprises the following steps:

[0050] S11. Add 0.142g of β-cyclodextrin and 1.61g of ZrOCl to 50g of water respectively 2 .8H 2 O, then add 1.68g of NaHCO 3 And the ethylenediaminetetraacetic acid of 2.0g, obtain mixed solution after stirring for 40min;

[0051] S12, transfer the above-mentioned mixed solution into the autoclave, and heat-treat under the condition of 200°C for 6 hours;

[0052] S13. Take out the autoclave and age at room temperature for 8 hours, then separate the precipitate and wash it with deionized water. After drying or calcination, the micro / nanostructure ZrO 2 , the sample is then calcined at 700°C to obtain a tetragonal and monoclinic mixed crystal phase micro / nanostructure ZrO 2 . The resulting sample was analyzed for morphology and crystal phase with a Japanese S-4800 scanning electron microscope and a German BrukerAXS D8ADVANCE X-ray diffractometer. The results are shown in figure 1 .

[0053] from figure 1 (a,...

Embodiment 2

[0055] The preparation method comprises the following steps:

[0056] S21, add 0.142g of β-cyclodextrin and 1.61g of ZrOCl in 30g of water 2 .8H 2 O, after stirring for 20min, make solution A; then add 1.68g of NaHCO in 20g of water 3 and 2.0g of EDTA, after stirring for 20min, it was made into solution B; after mixing the two solutions of A and B, they were fully stirred to obtain a mixed solution;

[0057] S22, transfer the above mixed solution into the autoclave, heat treatment at 200°C for 8 hours;

[0058] S23. Take out the autoclave and age at room temperature for 12 hours, then separate the precipitate and wash it with deionized water, dry or calcinate to obtain the micro / nanostructure ZrO 2 .

[0059] The resulting sample was analyzed for morphology and crystal phase with a Japanese S-4800 scanning electron microscope and a German BrukerAXS D8ADVANCE X-ray diffractometer. The results are shown in figure 2 .

[0060] from figure 2 (a, b, c) It can be seen that ...

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Abstract

The invention discloses ZrO2 with a micro / nano structure and a preparation method of ZrO2. ZrO2 is a multi-layer ZrO2 mesoporous microsphere which has a tertiary structure: an about 10-20 nm ZrO2 nano particle is used as a primary unit to be assembled into an about 100-200 nm ZrO2 nano sphere; the ZrO2 nano sphere as a secondary structure unit is assembled again into 1.0-2.0 micrometer ZrO2 microsphere. Beta-cyclodextrin and EDTA (edetic acid) are used as self-assembling mediums, the multi-layer ZrO2 microsphere with the micro / nano structure is prepared by using a beta-cyclodextrin inclusion and steric hindrance effect and an EDTA complexing action and adopting a hydrothermal method, favorably crystallized tetragonal zirconia can be obtained, without high-temperature calcinations, tetragonal and monoclinal mixed phase zirconia can be obtained after high-temperature calcinations, the preparation method is simple and novel, and the conditions are controllable.

Description

technical field [0001] The present invention relates to complex multi-level structure ZrO 2 preparation, specifically involving a micro / nanostructured ZrO 2 and its preparation method. Background technique [0002] ZrO 2 It is an important inorganic material. In addition to good optical, thermal, electrical, chemical and mechanical properties, it also has excellent surface properties, such as having both surface acidic and basic sites and redox properties. It is the only one A metal oxide that combines acidity, alkalinity and redox. In addition, it also has excellent ion exchange capacity, good thermal and chemical stability, high refractive index and low light absorption, so it has attracted much attention in the fields of catalysis, adsorption, optics, and environmental governance. But conventional ZrO 2 Small specific surface area, underdeveloped pores, and irregular pore size changes limit its excellent performance. Nano-ZrO 2 The application space in the field of...

Claims

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Application Information

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IPC IPC(8): C01G25/02B82Y30/00
CPCC01G25/02C01P2002/72C01P2004/03C01P2004/32C01P2004/64
Inventor 杨晓辉徐彬冯海燕曾敏张雪红
Owner SHIJIAZHUANG UNIVERSITY
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