CN103818957A - Method for preparing chip-like hollow zirconium oxide powder through water quenching process - Google Patents
Method for preparing chip-like hollow zirconium oxide powder through water quenching process Download PDFInfo
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- CN103818957A CN103818957A CN201410098561.XA CN201410098561A CN103818957A CN 103818957 A CN103818957 A CN 103818957A CN 201410098561 A CN201410098561 A CN 201410098561A CN 103818957 A CN103818957 A CN 103818957A
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Abstract
The invention provides a method for preparing chip-like hollow zirconium oxide powder through a water quenching process and belongs to the nano-powder material field. The method is characterized by comprising the steps of: based on a water quenching process, by taking zirconium oxychloride as the raw material, heating to the range from 800 to 1000 DEG C and preserving heat for 0.2-1h, and carrying out water quenching, and then obtaining the chip-like hollow zirconium oxide powder, wherein the temperature of a water quenching solution ranges from 10 to 30 DEG C, the water quenching solution is a zirconium oxychloride solution or an ammonium hydroxide solution, and the PH value of the water quenching solution ranges from 8 to 10. The powder morphology is in chip form, and the diameter of the powder ranges from 10 to 20 microns and the length of the powder ranges from 50 to 200 microns; the powder is formed through directional arrangement of a strip-like hollow structure, and the strip-like hollow structure is composed of nano zirconium oxide which is compact in surface layer and loose inside; the granularity of the nano zirconium oxide ranges from 20 to 50nm, the pore diameter of the strip-like hollow structure ranges from 0.5 to 1 micron, and the wall thickness of the strip-like hollow structure ranges from 0.2 to 1 micron. The method is simple in process, safe to operate, low in calcination temperature and low in particle granularity.
Description
Technical field
The invention provides a kind of water quenching and prepare the method for wood fragments shape hollow Zirconium powder, belong to nano-powder material field.
Background technology
Zirconium dioxide is a kind of high temperature resistant, wear-resistant, corrosion resistant ceramic, and except being applied to traditional refractory materials and beramic color, it is also widely used in high-tech areas such as electronic ceramics, function ceramics and structural ceramicss.Different-shape structure, as nano wire, nanometer rod, nanometer sheet, micron film, micron bar, shows different physicalies, has in a lot of fields different application, and spherical nanoparticle is conducive to improve ceramic compactness; Nano wire has the ceramic toughness of the raising of utilizing; Platy shaped particle is conducive to improve toughness and heat-shock resistance; Hollow structure is conducive to the carrier as catalyzer.From at present both at home and abroad to nano level ZrO
2research, the nanometer ZrO of preparation
2spherical, bar-shaped and sheet that particle is mainly.Micron particle is mainly spherical.And wood fragments shape hollow Zirconium powder there is no report.
Summary of the invention
The object of this invention is to provide high, the simple to operate safety of a kind of efficiency, water quenching that calcining temperature is low and prepare the method for wood fragments shape hollow Zirconium powder, its technical scheme is:
Adopt water quenching, take zirconium oxychloride as raw material, be heated to 800～1000 ℃ of insulation 0.2～1 h, shrend, shrend solution temperature is 10～30 ℃, shrend solution is sodium hydroxide solution or ammonia soln, the pH value of shrend solution is 8～10, obtains wood fragments shape hollow Zirconium powder.Morphology microstructure is wood fragments shape, diameter is 10～20 μ m, length is 50～200 μ m, powder is that strip hollow structure aligns and forms, strip hollow structure is top layer densification, the nano zircite composition of internal defect, and nano zircite granularity is 20～50 nm, the bore dia of strip hollow structure is 0.5～1 μ m, and wall thickness is 0.2～1 μ m.
Compared with prior art, tool has the following advantages in the present invention:
The pattern of the powder that 1, prepared by the present invention is wood fragments shape, can use crack deflection, toughening ceramic;
2, the powder that prepared by the present invention, powder is that strip hollow structure aligns and forms, and strip hollow structure is top layer densification, and the nano zircite composition of internal defect, can improve ceramic thermal shock resistance;
3, the powder that prepared by the present invention, powder is that strip hollow structure aligns and forms, specific surface area is large, can serve as support of the catalyst;
4, the present invention prepares the method for wood fragments shape hollow Zirconium powder, and efficiency is high, simple to operate, safety.
Accompanying drawing explanation
Fig. 1 is the embodiment of the present invention is prepared powder XRD spectrum in 20 ℃ of shrends of 900 ℃ of calcinings;
Fig. 2 is the embodiment of the present invention is prepared powder SEM photo in 20 ℃ of shrends of 900 ℃ of calcinings.
Embodiment
Embodiment 1
Adopt water quenching, take zirconium oxychloride as raw material, be heated to 800 ℃ of insulation 0.2 h, shrend, shrend solution temperature is 10 ℃, and shrend solution is sodium hydroxide solution, and the pH value of sodium hydroxide solution is 8, obtains wood fragments shape hollow Zirconium powder.
Embodiment 2
Adopt water quenching, take zirconium oxychloride as raw material, be heated to 900 ℃ of insulation 0.5 h, shrend, shrend solution temperature is 20 ℃, and shrend solution is sodium hydroxide solution, and the pH value of sodium hydroxide solution is 10, obtains wood fragments shape hollow Zirconium powder.
Test by XRD, visible powder crystal type is monoclinic phase (see figure 1); Test by SEM, visible Zirconium powder is wood fragments shape, diameter is 10～20 μ m, length is 50～200 μ m, and powder is that strip hollow structure aligns and forms, and strip hollow structure is top layer densification, the nano zircite composition of internal defect, nano zircite granularity is 20～50 nm, and the bore dia of strip hollow structure is 0.5～1 μ m, and wall thickness is that 0.2～1 μ m(is shown in Fig. 2).
Embodiment 3
Adopt water quenching, take zirconium oxychloride as raw material, be heated to 1000 ℃ of insulation 1 h, shrend, shrend solution temperature is 30 ℃, and shrend solution is ammonia soln, and the pH value of ammonia soln is 9, obtains wood fragments shape hollow Zirconium powder.
Claims (1)
1. a water quenching is prepared the method for wood fragments shape hollow Zirconium powder, it is characterized in that: adopt water quenching, take zirconium oxychloride as raw material, be heated to 900～1100 ℃ of insulation 0.2～1 h, shrend, shrend solution temperature is 10～30 ℃, shrend solution is sodium hydroxide solution or ammonia soln, the pH value of shrend solution is 8～10, obtain wood fragments shape hollow Zirconium powder, morphology microstructure is wood fragments shape, diameter is 10～20 μ m, length is 50～200 μ m, powder is that strip hollow structure aligns and forms, strip hollow structure is top layer densification, the nano zircite composition of internal defect, nano zircite granularity is 20～50nm, the bore dia of strip hollow structure is 0.5～1 μ m, wall thickness is 0.2～1 μ m.
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| CN201410098561.XA CN103818957B (en) | 2014-03-17 | 2014-03-17 | Method for preparing chip-like hollow zirconium oxide powder through water quenching process |
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| CN201410098561.XA CN103818957B (en) | 2014-03-17 | 2014-03-17 | Method for preparing chip-like hollow zirconium oxide powder through water quenching process |
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| CN103818957A true CN103818957A (en) | 2014-05-28 |
| CN103818957B CN103818957B (en) | 2017-04-26 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105152180A (en) * | 2015-10-19 | 2015-12-16 | 山东理工大学 | Preparation process of hollow rod-like zirconium boride powder |
| CN108558397A (en) * | 2018-04-26 | 2018-09-21 | 西安建筑科技大学 | A kind of preparation method, cenosphere and the application of high-purity zirconia cenosphere |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US3749763A (en) * | 1971-08-03 | 1973-07-31 | Humphreys Corp | Processing of silicate ores and product thereof |
| JPS5978928A (en) * | 1982-10-25 | 1984-05-08 | Agency Of Ind Science & Technol | Manufacture of zirconia powder |
| JPS62212225A (en) * | 1986-03-11 | 1987-09-18 | Nippon Shokubai Kagaku Kogyo Co Ltd | Production of zirconia-containing fine powder |
| CN101851005A (en) * | 2010-05-17 | 2010-10-06 | 山东理工大学 | Preparation method of high-dispersion zirconium oxide nano powder |
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2014
- 2014-03-17 CN CN201410098561.XA patent/CN103818957B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3749763A (en) * | 1971-08-03 | 1973-07-31 | Humphreys Corp | Processing of silicate ores and product thereof |
| JPS5978928A (en) * | 1982-10-25 | 1984-05-08 | Agency Of Ind Science & Technol | Manufacture of zirconia powder |
| JPS62212225A (en) * | 1986-03-11 | 1987-09-18 | Nippon Shokubai Kagaku Kogyo Co Ltd | Production of zirconia-containing fine powder |
| CN101851005A (en) * | 2010-05-17 | 2010-10-06 | 山东理工大学 | Preparation method of high-dispersion zirconium oxide nano powder |
Non-Patent Citations (3)
| Title |
|---|
| MASAHIRO YOSHIMURA ET AL.: "Hydrothermal synthesis of crystallized nano-particles of rare earth-doped zirconia and hafnia", 《MATERIALS CHEMISTRY AND PHYSICS》 * |
| 李霞等: "液相法制备ZrO2超微粉末的研究进展", 《中国陶瓷》 * |
| 王焕英等: "化学沉淀法制备纳米氧化锆的研究", 《河北师范大学学报(自然科学版)》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105152180A (en) * | 2015-10-19 | 2015-12-16 | 山东理工大学 | Preparation process of hollow rod-like zirconium boride powder |
| CN108558397A (en) * | 2018-04-26 | 2018-09-21 | 西安建筑科技大学 | A kind of preparation method, cenosphere and the application of high-purity zirconia cenosphere |
| CN108558397B (en) * | 2018-04-26 | 2021-02-09 | 西安建筑科技大学 | Preparation method of high-purity zirconia cenospheres, cenospheres and application |
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| CN103818957B (en) | 2017-04-26 |
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