CN103922399B - A kind of preparation method of zirconia nanopowder ball - Google Patents
A kind of preparation method of zirconia nanopowder ball Download PDFInfo
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Abstract
A preparation method for zirconia nanopowder ball, is dissolved in 5mmol ~ 10mmol metal zirconium compd A in 10ml ~ 100ml organic compound alcoholic solvent B and obtains solution C; 5mmol ~ 10mmol water is added in 500ml organic compound alcoholic solvent B and obtain solution D; Enough solution C is added in enough solution D and obtains solution E, and stir 1 ~ 3 hour; The solution E obtained is carried out eccentric cleaning, is precipitated and is scattered in solvent B and obtain zirconia nanopowder ball solution; The present invention is achieved by rational technique and at room temperature synthesizes the uniform zirconia nanopowder ball of appearance and size, and can prepare on a large scale.
Description
[technical field]
The present invention relates to a kind of preparation technology of zirconia nanopowder ball, especially relate to a kind of preparation method of zirconia nanopowder ball at room temperature.
[background technology]
Known, zirconium white has fusing point and boiling point is high, hardness is tall and big, then have the advantageous properties such as electroconductibility under high temperature for isolator under normal temperature; So zirconium white conduct, therefore one of stupalith received much concern in recent years is become, the ceramic component made of Zirconium powder and ceramic coating, there is the feature of wear-resistant, corrosion-resistant, high temperature resistant and high strength, high tenacity, high rigidity, contain all essential domains or civil area obtains application in Aeronautics and Astronautics, boats and ships, nuclear industry, machinery, metallurgy, electric power and national defense and military etc.And nanometer zirconium oxide ceramic coating, due to the existence of size effect and a large amount of crystal boundary, there is the performance more superior than conventional oxidation zirconium coating; As: microstructure crystal grain is piled up closely, void content bonding properties that is low, coating is better, therefore, has more wide application prospect.The key preparing high-performance nano coating is preparation nanostructure spherical powder material.For meeting the requirement of spraying coating process, the particles size and distribution of powder body material, shape and degree of mobilization are all important influence factors.
At present, the preparation method of Zirconium powder comprises solid phase method, vapor phase process and liquid phase method.Wherein, solid phase method and vapor phase process need accurate equipment, and combined coefficient compared with low, energy consumption large, be not suitable for a large amount of industrial production.Liquid phase method has coprecipitation method, hydrothermal method, sol-gel method, microemulsion method etc.Wherein, the earliest, reaction process is simple, production cost is lower in coprecipitation method exploitation, but usually need to adopt high-temperature calcination to obtain nano-powder in the later stage, not only energy consumption is high, and particle size is reunited greatly, easily, is difficult to obtain required size, the uniform nano-powder of pattern.Hydrothermal method, sol-gel method, microemulsion method are the preparation methods of Application and Development in recent years, and its powder quality prepared is better, but production technique and processing units are comparatively complicated, and especially production process is more, is unfavorable for scale operation.
Chinese patent " application number, CN200910018300.1; The applying date, on September 11st, 2009 " disclose a kind of production method of nano zircite; this patent application is obtained by reacting precipitated zirconium hydroxide by zirconium saline solution and alkaline precipitating agent; again through filtering, washing, dehydration, after drying; calcining obtains Zirconium powder, and diameter of particle is 10 ~ 80 nanometers; Unfortunately, the method needs through high temperature (500 ~ 1300 DEG C) calcining, and the powder size of acquisition is uneven, finds that the acquisition thing nano zircite of the method easily hard aggregation occurs through overtesting.
[summary of the invention]
For overcoming the deficiency that prior art exists, the invention provides a kind of preparation method of zirconia nanopowder ball, the present invention is achieved by rational technique and at room temperature synthesizes the uniform zirconia nanopowder ball of appearance and size, and can prepare on a large scale.
For achieving the above object, the present invention adopts following technical scheme:
A preparation method for zirconia nanopowder ball, comprises the steps:
1), 5mmol ~ 10mmol metal zirconium compd A is dissolved in 10ml ~ 100ml organic compound alcoholic solvent B obtains solution C;
2), 5mmol ~ 10mmol water is added in 500ml organic compound alcoholic solvent B and obtain solution D;
3), by enough solution C add in enough solution D and obtain solution E, and stir 1 ~ 3 hour;
4) solution E, by step 3) obtained carries out eccentric cleaning, is precipitated and is scattered in solvent B to obtain zirconia nanopowder ball solution.
The preparation method of described zirconia nanopowder ball, in described step 1), metal zirconium compd A is any one in following material: Zircosol ZN, basic zirconium chloride, zirconium acetate, methyl ethyl diketone zirconium, zirconyl carbonate, zirconium chloride, zirconium-n-propylate, zirconium-n-butylate.
The preparation method of described zirconia nanopowder ball, the solvent B in described step 1) is the one in following material: polyvinyl alcohol, polyoxyethylene glycol, glycerol, ethanol, ethylene glycol, propyl carbinol, methyl alcohol, isopropylcarbinol, Virahol.
The preparation method of described zirconia nanopowder ball, in described step 1), in solution C, the concentration of metal zirconium compd A is 0.01mM to 1M.
The preparation method of described zirconia nanopowder ball, described step 2) in solution D the concentration of water be 0.01mM to 1M.
The preparation method of described zirconia nanopowder ball, temperature required in described step 3) is room temperature.
The preparation method of described zirconia nanopowder ball, the churning time in described step 3) is 5 minutes to 5 hours.
Owing to have employed technique scheme, of the present invention have following beneficial effect:
The preparation method of zirconia nanopowder ball of the present invention, is dissolved in solvent B(alcohol by metal zirconium compd A) middle formation solution C; Water is added in solvent B and form solution D; Solution C is added in solution D and forms solution E, and stir required time; Eccentric cleaning is carried out to solution E, is precipitated and is scattered in solvent B and obtain zirconia nanopowder ball solution.Relative to additive method, method of the present invention is simple, environmental friendliness, appearance and size are controlled and can prepare on a large scale; The present invention is achieved by rational technique and at room temperature synthesizes appearance and size uniform zirconia nanopowder ball, and method is simple, be easy to control, environmental friendliness and preparing on a large scale.
[accompanying drawing explanation]
Fig. 1 is the stereoscan photograph of zirconia nanopowder ball of the present invention;
[embodiment]
Can explain the present invention in more detail by the following examples, the present invention is not limited to the following examples, discloses object of the present invention and is intended to protect all changes and improvements in the scope of the invention;
Following embodiment all can obtain zirconia nanopowder ball described in accompanying drawing 1.
Embodiment 1
By 10mmolZrO (NO
3)
2be dissolved in 100ml Virahol, form solution C.Then 10mmol water is added in 500ml Virahol, form solution D.Solution C is added in solution D, stir 1 hour.And then eccentric cleaning, obtain zirconia nanopowder ball.
Embodiment 2
By 10mmolZrO (Cl)
2be dissolved in 90ml glycerol, form solution C.Then 10mmol water is added in 500ml Virahol, form solution D.Solution C is added in solution D, stir 1 hour.And then eccentric cleaning, obtain zirconia nanopowder ball.
Embodiment 3
By 5mmolZrO (NO
3)
2be dissolved in 80ml Virahol, form solution C.Then 10mmol water is added in 500ml Virahol, form solution D.Solution C is added in solution D, stir 2 hours.And then eccentric cleaning, obtain zirconia nanopowder ball.
Embodiment 4
10mmol zirconium acetate is dissolved in 100ml Virahol, forms solution C.Then 5mmol water is added in 500ml Virahol, form solution D.Solution C is added in solution D, stir 1.5 hours.And then eccentric cleaning, obtain zirconia nanopowder ball.
Embodiment 5
By 8mmolZrO (NO
3)
2be dissolved in 100ml propyl carbinol, form solution C.Then 10mmol water is added in 500ml Virahol, form solution D.Solution C is added in solution D, stir 1 hour.And then eccentric cleaning, obtain zirconia nanopowder ball.
Embodiment 6
10mmol methyl ethyl diketone zirconium is dissolved in 10ml Virahol, forms solution C.Then 10mmol water is added in 500ml Virahol, form solution D.Solution C is added in solution D, stir 1 hour.And then eccentric cleaning, obtain zirconia nanopowder ball.
Embodiment 7
10mmol methyl ethyl diketone zirconium is dissolved in 100ml propyl carbinol, forms solution C.Then 8mmol water is added in 500ml Virahol, form solution D.Solution C is added in solution D, stir 2 hours.And then eccentric cleaning, obtain zirconia nanopowder ball.
Embodiment 8
By 10mmolZrO (NO
3)
2be dissolved in 100ml Virahol, form solution C.Then 10mmol water is added in 450ml Virahol, form solution D.Solution C is added in solution D, stir 1 hour.And then eccentric cleaning, obtain zirconia nanopowder ball.
Embodiment 9
By 10mmolZrO (NO
3)
2be dissolved in 100ml glycerol, form solution C.Then 10mmol water is added in 480ml Virahol, form solution D.Solution C is added in solution D, stir 1 hour.And then eccentric cleaning, obtain zirconia nanopowder ball.
Embodiment 10
10mmol methyl ethyl diketone zirconium is dissolved in 100ml Virahol, forms solution C.Then 5mmol water is added in 500ml Virahol, form solution D.Solution C is added in solution D, stir 3 hours.And then eccentric cleaning, obtain zirconia nanopowder ball.
Part not in the detailed description of the invention is prior art.
Claims (2)
1. a preparation method for zirconia nanopowder ball, is characterized in that: comprise the steps:
1), 5mmol ~ 10mmol metal zirconium compd A is dissolved in 10ml ~ 100ml organic compound alcoholic solvent B obtains solution C;
2), 5mmol ~ 10mmol water is added in 500ml organic compound alcoholic solvent B and obtain solution D;
3), at room temperature by enough solution C add in enough solution D and obtain solution E, and stir 5 minutes to 5 hours;
4) solution E, by step 3) obtained carries out eccentric cleaning, is precipitated and is scattered in solvent B to obtain zirconia nanopowder ball solution;
Wherein solvent B is the one in following material: polyvinyl alcohol, polyoxyethylene glycol, glycerol, ethanol, ethylene glycol, propyl carbinol, methyl alcohol, isopropylcarbinol, Virahol.
2. the preparation method of zirconia nanopowder ball according to claim 1, is characterized in that: in described step 1), metal zirconium compd A is any one in following material: Zircosol ZN, basic zirconium chloride, zirconium acetate, methyl ethyl diketone zirconium, zirconyl carbonate, zirconium chloride, zirconium-n-propylate, zirconium-n-butylate.
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| CN106832304B (en) * | 2017-03-03 | 2020-02-04 | 苏州图纳新材料科技有限公司 | Preparation method of water-soluble zirconia ceramic precursor and solution thereof |
| CN109110809A (en) * | 2018-08-03 | 2019-01-01 | 长江大学 | A kind of composite cathode material for lithium ion cell ZrO2And preparation method thereof |
| CN110217818A (en) * | 2019-06-13 | 2019-09-10 | 中国科学院广州地球化学研究所 | Uniform particle size zirconium dioxide nanosphere and its film and preparation method |
| CN111128023B (en) * | 2019-12-23 | 2022-01-18 | 华南理工大学 | Flexible substrate structure with adjustable toughness and preparation method thereof |
| CN113307635A (en) * | 2021-05-24 | 2021-08-27 | 中国船舶重工集团公司第七二五研究所 | Method for directly titrating and forming ceramic microspheres through gel casting of track |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1477060A (en) * | 2003-06-09 | 2004-02-25 | 清华大学 | Method for preparing nano-grade spherical zirconium oxide powder body |
| CN102249304A (en) * | 2010-05-21 | 2011-11-23 | 张永昶 | Method for preparing spherical nanometer zirconium dioxide |
| CN103588246A (en) * | 2012-08-13 | 2014-02-19 | 南宁市鼎发粉末冶金有限责任公司 | Preparation process for nano zirconia powder |
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| KR100544628B1 (en) * | 2003-03-07 | 2006-01-23 | 한국화학연구원 | Method for Continuous Preparation of Nano-sized Zirconia Hydrates Sol |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1477060A (en) * | 2003-06-09 | 2004-02-25 | 清华大学 | Method for preparing nano-grade spherical zirconium oxide powder body |
| CN102249304A (en) * | 2010-05-21 | 2011-11-23 | 张永昶 | Method for preparing spherical nanometer zirconium dioxide |
| CN103588246A (en) * | 2012-08-13 | 2014-02-19 | 南宁市鼎发粉末冶金有限责任公司 | Preparation process for nano zirconia powder |
Non-Patent Citations (1)
| Title |
|---|
| Hollow mesoporous zirconia nanocontainers for storing and controlled releasing of corrosion inhibitors;Arunchandran Chenan et al.;《Ceramics International》;20140317;第40卷;10457-10463 * |
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