Method for preparing zirconium dioxide ceramic microspheres with microfluid device

A microfluidic device, zirconium dioxide technology, applied in the field of material synthesis and forming, can solve the problem of difficult preparation of ceramic microspheres, and achieve the effects of preventing coalescence and adhesion, simple structure and good size consistency

Active Publication Date: 2013-01-30
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, monodisperse ceramic microspheres with high sphericity are still difficult to prepare despite great demand in engineering and energy fields.

Method used

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  • Method for preparing zirconium dioxide ceramic microspheres with microfluid device
  • Method for preparing zirconium dioxide ceramic microspheres with microfluid device
  • Method for preparing zirconium dioxide ceramic microspheres with microfluid device

Examples

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preparation example Construction

[0024] Using a microfluidic device, the zirconia precursor sol is wrapped with a mesophase fluid to form double-emulsion droplets. Using the double emulsion structure as a microreactor, adding an alkaline solution to the outside of the droplet triggers the reaction of the encapsulated zirconia precursor sol to form white gel microspheres. Zirconia ceramic microspheres can be obtained by sintering the white gel microspheres. Concrete preparation method comprises the following steps:

[0025] 1) Prepare the microchannel device: use the glass slide 5 as the substrate, insert the conical incident tube 1 and the conical collecting tube 2 from both ends of the square tube and arrange them coaxially, the two conical openings are opposite and leave a gap, and the conical opening of the incident tube is Smaller than the taper opening of the collection tube, the two ends of the square tube are respectively bonded with needles 4, the needles are bonded to the substrate, and the needles ...

Embodiment 1

[0035] Put the zirconia precursor gel solution, silicone oil, and 10wt% polyvinyl alcohol aqueous solution into the injection syringe respectively and connect the inner phase fluid, the intermediate phase fluid, and the continuous phase fluid inlet of the microfluidic device, and then load the injection syringe into the Digitally controlled flow on the pump.

[0036] Adjust the internal phase fluid flow rate to 200 μL / h, the interphase fluid flow rate to 450 μL / h, and the continuous phase fluid flow rate to 3500 μL / h. The outlet of the collection tube is connected to a PE-5 hose. After the droplet formation is stable, use a petri dish filled with a continuous phase fluid to collect the droplet. After a sufficient number of droplets had been collected, the Petri dish was transferred to a water bath and heated at 70°C for 40 minutes. After the heating, the same volume of ammonia water with a concentration of 2.5 mol / L as the continuous phase fluid was added to the petri dish, a...

Embodiment 2

[0038] The zirconia precursor sol solution, silicone oil, and 13wt% polyvinyl alcohol aqueous solution were respectively loaded into the injection syringe and connected to the inner phase fluid, intermediate phase fluid, and continuous phase fluid inlet of the microfluidic device, and then the injection syringe was loaded on the Digitally controlled flow on the pump. Adjust the internal phase fluid flow to 300 μL / h, the interphase fluid flow to 850 μL / h, and the continuous phase fluid flow to 3200 μL / h. The outlet of the collection tube is connected to a PE-5 hose. After the droplet formation is stable, use a petri dish filled with a continuous phase fluid to collect the droplet. After a sufficient number of droplets had been collected, the Petri dish was transferred to a water bath and heated at 80°C for 30 minutes. After heating, add ammonia water with a concentration of 4.5 mol / L in the same volume as the continuous phase fluid into the petri dish, and place it until white...

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Abstract

The invention relates to a method for preparing zirconium dioxide ceramic microspheres with a microfluid device, belonging to the technical field of material synthesis and formation. The method comprises the following steps: by using zirconium dioxide precursor sol as an inner phase fluid, an oily solution as an intermediate phase fluid and an aqueous solution as a continuous phase fluid, preparing monodisperse water-in-oil-in-water double-emulsion drops with a microfluid device by regulating the flow rates of the three phases of fluids, adding an alkaline solution into the continuous phase to initiate the gel reaction, cleaning and drying the gel microspheres obtained by the gel reaction, and sintering to obtain the ZrO2 ceramic microspheres. The zirconium dioxide ceramic microspheres prepared by the method have the advantages of high sphericity and uniform dimension; on the micrometer level, the action of surface tension of the zirconium dioxide ceramic microspheres is far larger than the deformation generated by gravity; and the reaction synthesis on the sol-gel system by using the double-emulsion drops as the template has universality, thereby having potential application prospects in the nuclear fuel preparation.

Description

technical field [0001] The invention relates to a method for preparing zirconia ceramic microspheres by using a microfluidic device built with a glass capillary, and belongs to the technical field of material synthesis and forming. Background technique [0002] ZrO 2 Ceramic materials have excellent high temperature resistance, wear resistance, and chemical corrosion resistance, and are widely used as reinforcing agents in cutting tools and structural materials. The material also has semiconductor properties, bio-affinity, and oxygen sensitivity, so it is also used to make piezoelectric ceramics, recording materials, etc. In addition, ZrO 2 Ceramics are now also used as templates to develop UOs that increase reaction efficiency and safety 2 Microspheres as a next-generation nuclear energy material. Therefore, ZrO 2 Ceramic microspheres are in great demand in fields such as engineering, biology, and energy. [0003] Traditional methods such as vibration dispersion, stir...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/48C04B35/624C04B35/626
Inventor 陈皓生张磊刘兵郝少昌
Owner TSINGHUA UNIV
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