CN103922399A - Preparation method of zirconium oxide nanospheres - Google Patents
Preparation method of zirconium oxide nanospheres Download PDFInfo
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- CN103922399A CN103922399A CN201410118558.XA CN201410118558A CN103922399A CN 103922399 A CN103922399 A CN 103922399A CN 201410118558 A CN201410118558 A CN 201410118558A CN 103922399 A CN103922399 A CN 103922399A
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Abstract
The invention relates to a preparation method of zirconium oxide nanospheres. The preparation method comprises the following steps: dissolving 5-10mmol of a zirconium compound A in 10-100ml of an organic compound alcohol solvent B to obtain a solution C; adding 5-10mmol of water into 500ml of the organic compound alcohol solvent B to obtain a solution D; adding a sufficient solution C into the sufficient solution D to obtain a solution E and stirring for 1-3 hours; and centrifugalizing the obtained solution E to obtain a precipitate, cleaning, and dispersing the precipitate in the solvent B to obtain the zirconium oxide nanosphere solution. The preparation method synthesizes the zirconium oxide nanospheres with uniform shape and size at room temperature through a reasonable process, and the zirconium oxide nanospheres can be prepared on a large scale.
Description
[technical field]
The present invention relates to a kind of preparation technology of zirconium white nanometer ball, especially relate to a kind of preparation method of zirconium white nanometer ball at room temperature.
[background technology]
Known, zirconium white has fusing point and boiling point is high, hardness is tall and big, for isolator high temperature is next, have the advantageous properties such as electroconductibility under normal temperature; So zirconium white conduct, therefore become one of stupalith receiving much concern in recent years, ceramic component and the ceramic coating of Zirconium powder, made, the feature with wear-resistant, corrosion-resistant, high temperature resistant and high strength, high tenacity, high rigidity, contains 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, the existence due to size effect and a large amount of crystal boundaries, has the performance more superior than conventional oxidation zirconium coating; As: microstructure crystal grain is piled up closely, void content bonding properties low, coating is better etc., therefore, has more wide application prospect.The key of preparing high-performance nano coating is preparation nanostructure spherical powder material.For meeting the requirement of spraying coating process, the particle diameter of powder body material and distribution thereof, 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, coprecipitation method is developed the earliest, and reaction process is simple, production cost is lower, but conventionally in the later stage, need to adopt high-temperature calcination to obtain nano-powder, not only energy consumption is high, and particle size greatly, easily reunites, and 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 of preparing 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 " a kind of production method of nano zircite disclosed; this patent application is reacted with alkaline precipitating agent by zirconium saline solution and is obtained zirconium hydroxide and precipitate; again through filtering, washing, dehydration, dry after; calcining obtains Zirconium powder, and diameter of particle is 10～80 nanometers; Not enough, the method need to be passed through high temperature (500～1300 ℃) calcining, and the powder size of obtaining is uneven, finds that hard aggregation easily occurs the thing nano zircite that obtains of the method through overtesting.
[summary of the invention]
For overcoming the deficiency of prior art existence, the invention provides a kind of preparation method of zirconium white nanometer ball, the present invention has realized the at room temperature synthetic uniform zirconium white nanometer ball of appearance and size by rational technique, and can prepare on a large scale.
For achieving the above object, the present invention adopts following technical scheme:
A preparation method for zirconium white nanometer ball, comprises the steps:
1), 5mmol～10mmol metal zirconium compd A is dissolved in 10ml～100ml organic compound alcoholic solvent B and obtains solution C;
2), 5mmol～10mmol water is added in 500ml organic compound alcoholic solvent B and obtains solution D;
3), enough solution C are added in enough solution D and obtain solution E, and stir 1～3 hour;
4), solution E that step 3) is obtained carries out eccentric cleaning, be precipitated and be scattered in solvent B, to obtain zirconium white nanometer ball solution.
The preparation method of described zirconium white nanometer 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 zirconium white nanometer ball, the solvent B in described step 1) is a kind of in following material: polyvinyl alcohol, polyoxyethylene glycol, glycerol, ethanol, ethylene glycol, propyl carbinol, methyl alcohol, isopropylcarbinol, Virahol.
The preparation method of described zirconium white nanometer 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 zirconium white nanometer ball, described step 2) in, in solution D, the concentration of water is 0.01mM to 1M.
The preparation method of described zirconium white nanometer ball, temperature required in described step 3) is room temperature.
The preparation method of described zirconium white nanometer ball, the churning time in described step 3) is 5 minutes to 5 hours.
Owing to having adopted technique scheme, of the present invention have a following beneficial effect:
The preparation method of zirconium white nanometer ball of the present invention, is dissolved in solvent B(alcohol by metal zirconium compd A) the middle solution C that forms; Water is added in solvent B and forms solution D; Solution C is added and in solution D, forms solution E, and stir required time; Solution E is carried out to eccentric cleaning, be precipitated and be scattered in and in solvent B, obtain zirconium white nanometer ball solution.With respect to additive method, method of the present invention is simple, environmental friendliness, appearance and size is controlled and can prepare on a large scale; The present invention has realized at room temperature the synthetic uniform zirconium white nanometer ball of appearance and size by rational technique, and method is simple, be easy to control, environmental friendliness and can prepare on a large scale.
[accompanying drawing explanation]
Fig. 1 is the stereoscan photograph of zirconium white nanometer ball of the present invention;
[embodiment]
By the following examples, can explain in more detail the present invention, 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 zirconium white nanometer ball described in accompanying drawing 1.
Embodiment 1
By 10mmol ZrO (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 zirconium white nanometer ball.
Embodiment 2
By 10mmol ZrO (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 zirconium white nanometer ball.
Embodiment 3
By 5mmol ZrO (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 zirconium white nanometer 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 zirconium white nanometer ball.
Embodiment 5
By 8mmol ZrO (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 zirconium white nanometer 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 zirconium white nanometer 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 zirconium white nanometer ball.
Embodiment 8
By 10mmol ZrO (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 zirconium white nanometer ball.
Embodiment 9
By 10mmol ZrO (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 zirconium white nanometer 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 zirconium white nanometer ball.
Part not in the detailed description of the invention is prior art.
Claims (7)
1. a preparation method for zirconium white nanometer 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 and obtains solution C;
2), 5mmol～10mmol water is added in 500ml organic compound alcoholic solvent B and obtains solution D;
3), enough solution C are added in enough solution D and obtain solution E, and stir 1～3 hour;
4), solution E that step 3) is obtained carries out eccentric cleaning, be precipitated and be scattered in solvent B, to obtain zirconium white nanometer ball solution.
2. the preparation method of zirconium white nanometer 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.
3. the preparation method of zirconium white nanometer ball according to claim 1, is characterized in that: the solvent B in described step 1) is a kind of in following material: polyvinyl alcohol, polyoxyethylene glycol, glycerol, ethanol, ethylene glycol, propyl carbinol, methyl alcohol, isopropylcarbinol, Virahol.
4. the preparation method of zirconium white nanometer ball according to claim 1, is characterized in that: in described step 1), in solution C, the concentration of metal zirconium compd A is 0.01mM to 1M.
5. the preparation method of zirconium white nanometer ball according to claim 1, is characterized in that: described step 2), in solution D, the concentration of water is 0.01mM to 1M.
6. the preparation method of zirconium white nanometer ball according to claim 1, is characterized in that: temperature required in described step 3) is room temperature.
7. the preparation method of zirconium white nanometer ball according to claim 1, is characterized in that: the churning time in described step 3) is 5 minutes to 5 hours.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106832304A (en) * | 2017-03-03 | 2017-06-13 | 苏州图纳新材料科技有限公司 | A kind of preparation method of zirconium oxide presoma and its solution |
| 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 |
| CN111128023A (en) * | 2019-12-23 | 2020-05-08 | 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 |
Citations (4)
| 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 |
| JP2006503790A (en) * | 2003-03-07 | 2006-02-02 | コリアリサーチインスティテュートオブケミカルテクノロジー | Continuous production method of zirconia hydrate nanoparticle sol |
| 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 |
-
2014
- 2014-03-27 CN CN201410118558.XA patent/CN103922399B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006503790A (en) * | 2003-03-07 | 2006-02-02 | コリアリサーチインスティテュートオブケミカルテクノロジー | Continuous production method of zirconia hydrate nanoparticle sol |
| 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 |
|---|
| ARUNCHANDRAN CHENAN ET AL.: "Hollow mesoporous zirconia nanocontainers for storing and controlled releasing of corrosion inhibitors", 《CERAMICS INTERNATIONAL》, vol. 40, 17 March 2014 (2014-03-17), pages 10457 - 10463, XP028651280, DOI: 10.1016/j.ceramint.2014.03.016 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106832304A (en) * | 2017-03-03 | 2017-06-13 | 苏州图纳新材料科技有限公司 | A kind of preparation method of zirconium oxide presoma and its solution |
| 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 |
| CN111128023A (en) * | 2019-12-23 | 2020-05-08 | 华南理工大学 | Flexible substrate structure with adjustable toughness and preparation method thereof |
| 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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| CN103922399B (en) | 2016-01-20 |
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