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A kind of preparation method of monoclinic zirconia nano product

A zirconia and product technology, which is applied in the field of preparation of monoclinic zirconia nano products, can solve the problems of single type of zirconium source raw materials, complex synthesis process, increased synthesis cost, etc., and achieves good application prospects, high purity, and easy operation and control. Effect

Active Publication Date: 2020-10-23
GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, in the traditional process of synthesizing zirconia nanopowder by the liquid phase method, the types of zirconium source materials used are relatively single, and new high-quality and cheap zirconium source materials need to be further developed; at the same time, a variety of inorganic and Organic reagents, some reagents are relatively rare and expensive, which increases the synthesis cost and makes the synthesis process too complicated. It is also urgent to simplify the synthesis process and reduce the synthesis cost; finally, the traditionally synthesized nano-zirconia is mostly monoclinic and tetragonal Or a mixture of cubic phases, the synthesis of uniform, pure nano-zirconia of a certain crystal form is a technology that needs to be improved in the current process

Method used

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  • A kind of preparation method of monoclinic zirconia nano product
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  • A kind of preparation method of monoclinic zirconia nano product

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Effect test

Embodiment 1

[0038] The preparation method of the monoclinic zirconia nanopowder provided in this embodiment comprises the following steps:

[0039] (1) 0.48g ammonium fluozirconate ((NH 4 ) 2 ZrF 6 , purity 99%, West Asia reagent, the same below) was dissolved in 100L deionized water and fully dissolved to obtain a 0.02mol / L reaction solution. The high-temperature and high-pressure reactor is connected with a high-precision ultra-high pressure pressure gauge, a vent pipe and a stop valve. The high-temperature and high-pressure reactor has a metal shell, and a polytetrafluoroethylene lining is arranged in the metal shell. After the reactor is tightened , inject argon gas into the kettle through the ventilation pipe to a pressure of 50MPa, close the stop valve to stop the gas injection, heat the reaction kettle through a heating furnace, and set the reaction temperature to 200°C;

[0040] (2) After the temperature rises to 200°C, open the shut-off valve in step (1), continue to add argon...

Embodiment 2

[0047] The preparation method of the monoclinic zirconia nanopowder provided in this embodiment comprises the following steps:

[0048] (1) Dissolve 0.24g of ammonium fluozirconate in 100mL of deionized water to obtain a 0.01mol / L reaction solution. Put 5mL of the prepared reaction solution into a gold tube with a diameter of 4.5mm and seal it. Then put the gold tube into the Enter the high-temperature and high-pressure reactor, after tightening the reactor, inject argon gas into the reactor through the ventilation pipe to a pressure of 80MPa, close the stop valve to stop the gas injection, heat the reactor through a heating furnace, and set the reaction temperature to 250°C;

[0049] (2) After the temperature rises to 250°C, open the stop valve in step (1), continue to add argon to the pressure of 100MPa, and keep the reaction time for 12 hours. After the reaction is completed, use ice water to pour the reactor in step (1) to carry out Rapid cooling to room temperature;

[0...

Embodiment 3

[0054] The preparation method of the monoclinic zirconia nanopowder provided in this embodiment comprises the following steps:

[0055] (1) Dissolve 0.48g of ammonium fluozirconate in 100mL of deionized water to obtain a 0.02mol / L reaction solution, put the prepared reaction solution into a hydrothermal reactor, and place a flat gold sheet at the bottom of the reactor After tightening the reactor, inject argon gas into the reactor through the ventilation pipe to a pressure of 80MPa, close the stop valve to stop the gas injection, heat the reactor through a heating furnace, and set the reaction temperature to 250°C;

[0056] (2) After the temperature rises to 250°C, open the stop valve in step (1), continue to add argon to the pressure of 120MPa, and keep the reaction time for 10 hours. After the reaction is completed, use ice water to pour the reactor in step (1) to carry out Rapid cooling to room temperature;

[0057] (3) Open the reaction kettle in step (1), recover the res...

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Abstract

The invention discloses a preparation method of a monoclinic zirconia nano product. The preparation method is characterized by comprising the following steps: taking an ammonium fluorozirconate dilute solution as an initial raw material, placing the ammonium fluorozirconate dilute solution in a hydrothermal reaction kettle, then carrying out sealing, adjusting the temperature in the hydrothermal reaction kettle to be 200-500 DEG C, regulating the pressure to be 80-120 MPa, carrying out a self-hydrolysis reaction for 10-15 hours, rapidly carrying out cooling after the reaction is ended, opening the reaction kettle, taking out the residual solution, then collecting the sample, washing the sample, and drying the sample to obtain the monoclinic zirconia product, wherein the monoclinic zirconia product is monoclinic zirconia nano powder with uniform particle sizes or a monoclinic zirconia nano coated product. According to the preparation method, the ammonium fluorozirconate ((NH4)2ZrF6) is adopted as the raw material, and the monoclinic-phase zirconium oxide nano powder and a coating film of the monoclinic-phase zirconium oxide nano powder are synthesized through the single-reagent high-temperature hydrolysis reaction. In addition, the monoclinic-phase zirconium oxide nano powder particles are uniform in particle, large in specific surface area and high in purity.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials, and in particular relates to a preparation method of monoclinic zirconia nanometer products. Background technique [0002] Zirconia (ZrO 2 ) is a very important structural and functional material with excellent physical and chemical properties, such as high melting point (up to 2700 ° C), high boiling point, high hardness, small thermal conductivity, large thermal expansion coefficient and good particle size Electrical conductivity, and wear resistance, high temperature resistance, corrosion resistance and oxidation resistance. Since the 1980s, in addition to being used as a traditional refractory material and ceramic glaze, zirconia has also received more and more attention in the application of energy, environment and materials. Due to its tiny size, nano-zirconia is different from conventional materials in terms of optics, mechanics, thermodynamics and electromagnetics, so it is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G25/02B82Y40/00
CPCB82Y40/00C01G25/02C01P2002/82C01P2004/02C01P2004/03C01P2004/62C01P2004/64
Inventor 丁兴严海波刘灼瑜
Owner GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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