CN101844807B - Preparation method of platy hafnium oxide nano powder - Google Patents
Preparation method of platy hafnium oxide nano powder Download PDFInfo
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- CN101844807B CN101844807B CN2010101825910A CN201010182591A CN101844807B CN 101844807 B CN101844807 B CN 101844807B CN 2010101825910 A CN2010101825910 A CN 2010101825910A CN 201010182591 A CN201010182591 A CN 201010182591A CN 101844807 B CN101844807 B CN 101844807B
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Abstract
The invention provides a preparation method of platy hafnium oxide nano powder, belonging to the field of nano powder materials. The preparation method, which utilizes a solid phase method and takes hafnium tetrachloride and oxalic acid as raw materials, is characterized by comprising the following steps: mixing the two raw materials according to the mol ratio of 1:1-3, carrying out even ball milling, and then calcining for 2h at the temperature of 450-800 DEG C to obtain the platy hafnium oxide nano powder the thickness of which is about 10mm and the width of which is larger than 50nm. The platy hafnium oxide nano powder preparation method has simple process, safe operation, and low calcining temperature; and the platy hafnium oxide nano powder has small particles, and can be used as a platy thickening material.
Description
Technical field
The present invention provides a kind of preparation method of platy hafnium oxide nano powder, belongs to the nano-powder material field.
Background technology
Toughened zirconium oxide ceramic is a structural ceramic material of new generation, and it is to use the principle of transformation toughening to make ceramic highly malleablized, obtains zirconia ceramics high-strength, high-ductility.Hafnia has similar crystalline structure (monocline, pros and tetragonal structure) with zirconium white, and monoclinic form has minimum formation free energy and maximum volume, is the cryostatic stabilization phase; Zirconium white undergoes phase transition at 1200 ℃, changes tetragonal structure into, to 2710 ℃; By tetragonal phase converting is a cube phase, and hafnia undergoes phase transition at 1750 ℃, changes tetragonal structure into; To 2900 ℃, be a cube phase by tetragonal phase converting.Hafnia has higher transformation toughening temperature, helps in higher temperature as additive toughening ceramic material.
Flaky material (like graphite), utilization crack deflection, crackle bridging, platy shaped particle are extracted the effect toughening ceramic.If hafnia has sheet structure, when the toughening ceramic material, promptly having transformation toughening, to have sheet again toughness reinforcing, can better improve the toughening effect of pottery, but the preparation technology of platy hafnium oxide do not appear in the newspapers.
The preparation method report that has only the ball shaped nano hafnia at present: " liquid-phase precipitation method prepares HfO like the paper of Wu Zhihua etc.
2Nano-powder " adopt the ammonia water titration zirconium oxychloride, prepare the hafnium oxide powder of 10nm, to analyze through DSC-TG, its invert point is 593 ℃; Paper " preparation of nano-hafnium oxide powder and sign " the employing sodium hydroxide that Liu builds strong grade is precipitation agent; Polyoxyethylene glycol is a dispersion agent; Prepare the hafnium oxide powder less than 50nm, analyze through DSC-TG, its invert point is 649 ℃; 700 ℃ of calcinings generate monocline phase oxidation hafnium, and its crystal formation invert point is higher.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of efficient height, safety simple to operate, platy hafnium oxide nano powder that calcining temperature is low; It is characterized in that: adopt solid phase method; With hafnium tetrachloride and oxalic acid is raw material, and 1: 1 in molar ratio～3 with both mixing, and ball milling is even; At 450～800 ℃ of calcining 2h, promptly get platy hafnium oxide nano powder then.
The present invention compared with prior art has following advantage:
1, platy hafnium oxide nano powder can use crack deflection, crackle bridging, platy shaped particle to extract the effect toughening ceramic;
2, the present invention adopts solid reaction process synthesizing flaky hafnium oxide nano powder, and efficient is high, and is simple to operate, safety;
3, the hafnium oxide powder of the present invention's preparation has sheet structure, and loose reunion makes it have bigger specific surface area;
4, the present invention utilizes oxalic acid and hafnium tetrachloride low-temperature solid phase reaction, generates the oxalic acid zirconium, and pyrolytic decomposition prepares hafnia then, and the pyrolytic conversion temperature is low, and 405 ℃ promptly generate monocline phase oxidation hafnium, and calcining temperature is low.
Description of drawings
Fig. 1 is the DTA-TG curve of powder behind the ball milling of the present invention;
Fig. 2 is the XRD spectrum of the embodiment of the invention after 500 ℃ of calcinings;
Fig. 3 is the SEM photo of the embodiment of the invention after 500 ℃ of calcinings.
Embodiment
Embodiment 1
With hafnium tetrachloride and oxalic acid is raw material, and ball milling was even with both mixing in 1: 1 in molar ratio, at 800 ℃ of calcining 2h, promptly gets the hafnium oxide powder with nano-pore structure then.
With hafnium tetrachloride and oxalic acid is raw material, and ball milling was even with both mixing in 1: 2 in molar ratio, at 500 ℃ of calcining 2h, promptly gets the hafnium oxide powder with nano-pore structure then.
Through the DTA-TG curve, visible crystal formation invert point is 405 ℃ of (see figure 1)s; Through the XRD test, visible powder crystal type is a monocline phase (see figure 2); Through the SEM test, visible hafnium oxide powder thickness is about 10nm, and width is greater than the 500nm (see figure 3).
Embodiment 3
With hafnium tetrachloride and oxalic acid is raw material, and ball milling was even with both mixing in 1: 3 in molar ratio, at 450 ℃ of calcining 2h, promptly gets the hafnium oxide powder with nano-pore structure then.
Claims (1)
1. the preparation method of a platy hafnium oxide nano powder is characterized in that: adopting solid phase method, is raw material with hafnium tetrachloride and oxalic acid; 1: 1 in molar ratio～3 with both mixing; Ball milling is even, at 450～800 ℃ of calcining 2h, promptly gets platy hafnium oxide nano powder then.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101825910A CN101844807B (en) | 2010-05-17 | 2010-05-17 | Preparation method of platy hafnium oxide nano powder |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010101825910A CN101844807B (en) | 2010-05-17 | 2010-05-17 | Preparation method of platy hafnium oxide nano powder |
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| Publication Number | Publication Date |
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| CN101844807A CN101844807A (en) | 2010-09-29 |
| CN101844807B true CN101844807B (en) | 2012-04-25 |
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| CN2010101825910A Expired - Fee Related CN101844807B (en) | 2010-05-17 | 2010-05-17 | Preparation method of platy hafnium oxide nano powder |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2603788C1 (en) * | 2015-07-20 | 2016-11-27 | Федеральное государственное бюджетное учреждение науки Институт органического синтеза им. И.Я. Постовского Уральского отделения Российской академии наук (ИОС УрО РАН) | Method for production of hafnium dioxide nanorods |
| CN106745276B (en) * | 2017-01-24 | 2018-06-22 | 南昌大学 | A kind of preparation method of restoring tungsten oxide nanometer sheet |
| CN106745275B (en) * | 2017-01-24 | 2018-06-22 | 南昌大学 | A kind of preparation method of hydration tungstic trioxide nano-slice |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86104600A (en) * | 1985-07-03 | 1987-02-18 | 日产化学工业株式会社 | Flaky zirconia type fine crystals and production method thereof |
| EP0687246B1 (en) * | 1992-11-04 | 1998-04-01 | Egbert Dr. Brandau | Process for producing stabilised hafnium oxide powder or a hafnium oxide-containing powder |
| CN1749171A (en) * | 2004-09-13 | 2006-03-22 | 广东工业大学 | Medium-low temperature solid-solid reaction method for preparing nano grade cerium-zirconium composite oxide solid solution |
-
2010
- 2010-05-17 CN CN2010101825910A patent/CN101844807B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86104600A (en) * | 1985-07-03 | 1987-02-18 | 日产化学工业株式会社 | Flaky zirconia type fine crystals and production method thereof |
| EP0687246B1 (en) * | 1992-11-04 | 1998-04-01 | Egbert Dr. Brandau | Process for producing stabilised hafnium oxide powder or a hafnium oxide-containing powder |
| CN1749171A (en) * | 2004-09-13 | 2006-03-22 | 广东工业大学 | Medium-low temperature solid-solid reaction method for preparing nano grade cerium-zirconium composite oxide solid solution |
Non-Patent Citations (1)
| Title |
|---|
| 魏春城等.纳米氧化铪粉体的制备及表征.《中国陶瓷》.2009,第45卷(第7期),20-22. * |
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