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Preparation method of spherical zirconium silicate nano aggregate powder

A technology of nano-powder and zirconium silicate, which is applied in the direction of nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problem that it is difficult to show the performance advantages of nano-coating, the surface roughness of micron-spherical powder, the influence of Use performance and other issues to achieve the effect of eliminating the introduction of impurities, avoiding hard agglomeration, and reducing production costs

Inactive Publication Date: 2014-02-19
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the preparation process of agglomerate powder, the original nano-powder of zirconium silicate generally needs to go through processes such as calcination, spray granulation and high-temperature sintering. After the above-mentioned processes, most of the original nano-powder grains tend to grow It is a micron grain, so that the final agglomerate powder is in the micron scale. For example, under the action of sintering, a plurality of small nano-powder particles will stick together to form a micron spherical powder; zirconium silicate micron agglomerate powder When the powder is used as a raw material, there is almost no nanostructure in the coating structure prepared from it, and it is difficult to show the performance advantages of the nano-coating; at the same time, the surface of the micron spherical powder is generally loose and rough, and the bonding strength is low, which affects its performance. ; and the follow-up processing procedures of the prior art are too many and too complicated

Method used

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  • Preparation method of spherical zirconium silicate nano aggregate powder
  • Preparation method of spherical zirconium silicate nano aggregate powder
  • Preparation method of spherical zirconium silicate nano aggregate powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) 31.70g zirconium oxychloride octahydrate (ZrOCl 2 ·8H 2 O), 34.97g sodium metasilicate nonahydrate (Na 2 SiO 3 9H 2 O) Mix it with 500g deionized water as a raw material, separate the precipitate, wash it with deionized water, and dry it in an oven at 100°C, and the obtained powder is the precursor;

[0034] (2) Add 8.26g of mineralizing agent sodium fluoride (NaF) to 18g of precursor and mix with 1L of deionized water, put it into a 1.5L barrel reactor for hydrothermal reaction, the reaction time is 4h, and the reaction temperature is 180 ℃, the impurity-containing zirconium silicate powder is obtained, and the powder is softly agglomerated at this time;

[0035] (3) Mix 18g of impurity-containing zirconium silicate powder obtained in step (2) with 4L of deionized water, use an inorganic membrane separator to wash and filter to obtain a concentrated slurry, and the operating pressure of the inorganic membrane separator is 0.2MPa~0.25MPa, the washing temperatur...

Embodiment 2

[0046] (1) 41.98g of zirconium oxychloride octahydrate and 24.69g of sodium metasilicate nonahydrate were used as raw materials to make a mixed solution with 650g of deionized water. The precipitate was separated, washed with deionized water, and dried in an oven at 100°C. The obtained powder was Precursor.

[0047] (2) Add 10.94g of mineralizing agent sodium fluoride to 24g of precursor and mix with 1L of deionized water, put it into a 1.5L barrel reactor for hydrothermal reaction, the reaction time is 10h, and the reaction temperature is 380℃, the obtained Zirconium silicate powder with impurities, at this time, the powder is softly agglomerated;

[0048] (3) Mix 24g of impurity-containing zirconium silicate powder obtained in step (2) with 4L of deionized water, use an inorganic membrane separator to wash and filter to obtain a concentrated slurry, and the operating pressure of the inorganic membrane separator is 0.2MPa~0.25MPa, the washing temperature is 70℃~80℃, the memb...

Embodiment 3

[0059] (1) Mix 35.42g of zirconium oxychloride octahydrate and 31.25g of sodium metasilicate nonahydrate as raw materials with 500g of deionized water, separate the precipitate, wash with deionized water, and dry in an oven at 100°C, and the obtained powder is the precursor;

[0060] (2) Add 9.22g of mineralizing agent sodium fluoride and 1L of deionized water to 20g of the precursor, mix it with 1L of deionized water, put it into a 1.5L cylinder reactor for hydrothermal reaction, the reaction time is 6h, and the reaction temperature is 200℃, the obtained Zirconium silicate powder with impurities, at this time, the powder is softly agglomerated;

[0061] (3) Mix 20g of impurity-containing zirconium silicate powder obtained in step (2) with 4L of deionized water, use an inorganic membrane separator to wash and filter to obtain a concentrated slurry, and the operating pressure of the inorganic membrane separator is 0.2MPa~0.25MPa, the washing temperature is 70℃~80℃, the membrane...

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Abstract

The invention relates to a preparation method of spherical zirconium silicate nano aggregate powder, and belongs to the technical field of an inorganic material. The preparation method comprises the steps as follows: zirconium oxychloride and sodium metasilicate are mixed with water, precipitation is separated out, and washing and drying are performed to obtain a precursor; sodium fluoride and water are added into the precursor and reacts at the temperature of 180-380 DEG C for 4-10 hours to obtain zirconium silicate powder containing impurities; the zirconium silicate powder containing impurities is mixed with water and filtered and washed by an inorganic membrane separation device to obtain concentrated slurry, pie powder is obtained through pressure filtration, and zirconium silicate powder is obtained through drying; the zirconium silicate powder and absolute ethyl alcohol are mixed, and ground and emulsified in a colloid mill so as to obtain a mixed turbid liquid of the zirconium silicate nano powder and absolute ethyl alcohol; and the mixed turbid liquid is processed by a liquid powder feeder and inductive plasma spheroidization equipment, the zirconium silicate nano powder of the mixed turbid liquid is subjected to agglomeration, spheroidization and densification process to obtain the powder. The method is simple and low in cost, the spherical zirconium silicate nano aggregate powder can be directly prepared, and the purity quality is improved.

Description

technical field [0001] The present invention relates to a kind of zirconium silicate (ZrSiO 4 ) The preparation method of spherical nano aggregate powder belongs to the technical field of inorganic materials. Background technique [0002] With the development of aviation and aerospace technology, the operating temperature and pressure requirements of aircraft engine hot-end components and airframes continue to increase. Correspondingly, there are higher requirements for the high temperature resistance and oxidation resistance of the materials used in the hot end parts of the aircraft engine and the airframe. Zirconium silicate (ZrSiO 4 ) is a silicate compound with a tetragonal island structure. Compared with YSZ (yttria-stabilized zirconia), it has a higher refractive index, more excellent high-temperature phase structure stability, and better Chemical stability (such as acid and alkali corrosion resistance), excellent thermal shock resistance and oxidation resistance, b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/20B82Y30/00B82Y40/00
Inventor 柳彦博王全胜孙现凯马壮张锐
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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