CN101302361A - Preparation of zircite cladding iron oxide powder - Google Patents
Preparation of zircite cladding iron oxide powder Download PDFInfo
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- CN101302361A CN101302361A CNA2008100388238A CN200810038823A CN101302361A CN 101302361 A CN101302361 A CN 101302361A CN A2008100388238 A CNA2008100388238 A CN A2008100388238A CN 200810038823 A CN200810038823 A CN 200810038823A CN 101302361 A CN101302361 A CN 101302361A
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- iron oxide
- zircite
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- zirconium
- ferric oxide
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Abstract
The invention relates to a method for preparing a ferric oxide powder body coated with zirconia, which belongs to the coating material field. The method comprises the following steps that: nanometer ferric oxide particles are dispersed in a zirconic inorganic salt solution; a PH value of a dispersion system is adjusted through adding acid; and the temperature and the reaction time of the dispersion system are controlled in order that zirconium salt is hydrolyzed in a specific condition. The method can realize the coating on an ultrathin layer of the ferric oxide nanometer particles by the amorphous zirconia, thereby preparing a hetero-coating powder body with a nuclear shell structure; and the method has the advantages of simple process, easy control, no need of adding a surface active agent, etc. The prepared coated layer which is coated on particles is thin, can well maintain the shape and the nanometer property of the original particles and is convenient to popularize in industrialized production.
Description
Technical field
The present invention relates to a kind of preparation method of zircite cladding iron oxide powder, belong to the coating material field,
Background technology
In recent years; along with people are more and more higher to the performance requriements of material, concrete practical condition can not have been satisfied in original surface of most materials, therefore; necessary have some specific function particle to some and coat, thereby effectively protect its original nano-meter characteristic.
For guaranteeing dispersion of particles; oxidation-resistance; corrosion resistance; often require the protective layer about the surface of some superfine nano particles coating one deck 10nm; traditional nanoparticle cladding process generally all is to coat with organic polymer; or when preparing nanoparticle with metal-salt, coat, these existing cladding process always are difficult to satisfy when requiring in the face of these are new.
In these nanometers that coated, ferric oxide nano particles can be used as good pigment, coating, magnetic pipe recording material etc., is with a wide range of applications.Yet,, therefore, be easy to suffer erosion or cause thus and reunite and can not guarantee its dispersing characteristic because itself granularity is less.Traditional technology coats ferric oxide, mainly is it is embedded among the body material, and the material that obtains often has very big granularity, so just is difficult to guarantee the nanoparticle effect of itself.
In addition, evenly coat the layer of zirconia presoma, can effectively protect the surface of ferric oxide in iron oxide surface.Yet alkoxide hydrolysis commonly used not only needs to add tensio-active agent, and the zirconates precursor particle is difficult to prepare uniform coating layer owing to itself have very high chemically reactive, and cost is also relatively more expensive, also is unfavorable for suitability for industrialized production and popularization.
Summary of the invention
The present invention is directed to the difficult point of prior art, propose with zirconates as raw material, in the preparation method of iron oxide surface deposition one deck zirconium white presoma.This preparation method can be at the ultrafine unformed zirconia layer of surface deposition one deck of nano level ferric oxide particles.
The preparation method of the zircite cladding iron oxide powder that the present invention proposes, its concrete processing step is as follows:
(1) zirconium saline solution of configuration deposition precursor body, the concentration of zirconium saline solution is 0.1mmol/L～1.0mmol/L, the scope of the pH value of solution is 0～2;
The zirconates of selecting for use is Zircosol ZN, zirconium chloride, zirconium nitrate, zirconium oxychloride.
(2) ferric oxide particles is joined in the solution of above-mentioned zirconates, ultra-sonic dispersion 5～30 minutes, the grain diameter of the ferric oxide of selecting for use are 10nm～5 μ m.
(3) with above-mentioned dispersion system under the environment of heating in water bath, continue to stir 5 minutes～48 hours, the temperature of water-bath environment is 15～100 ℃.
(4) products therefrom is removed supernatant liquid through separating, and washing, dispersion and repeat number are inferior.
(5) above-mentioned product is done oven dry in 15～200 ℃ of vacuum, obtain zircite cladding iron oxide powder.
Method for coating provided by the present invention is a softening method, and the raw material that is coated is commercially available Fe
2O
3Nano-powder.Prepared powder characterizes the pattern and the structure of product through transmission electron microscope (TEM), scanning electronic microscope (SEM).Identify the elementary composition of coating product with energy spectrum analysis (EDS).
The present invention mainly by pH value, concentration of reactants and the temperature of reaction etc. of regulator solution, does not need to introduce tensio-active agent and organic solvent, and reaction conditions is simple, and production cost is low, is convenient to control.The coating layer of product is thinner, and thickness is even, and is active high, keeps original granule-morphology substantially.Can satisfy people at present to the needs of ferric oxide particles surface modification.
Description of drawings
Fig. 1 is the transmission electron microscope photo (TEM) of embodiment 1 zircite cladding iron oxide powder.
Fig. 2 is the high-resolution-ration transmission electric-lens photo (HRTEM) of embodiment 1 even zirconium white precursor layer.
Fig. 3 is the stereoscan photograph (SEM) of embodiment 2 zirconium white coated iron oxides.
Fig. 4 is the collection of illustrative plates (EDS) to the energy spectrum analysis of the shell that coats product.
Embodiment
Embodiment 1
At first prepare the aqueous solution of zirconium oxychloride: get eight hydration zirconium oxychloride (ZrOCl
28H
2O) 0.16g is dissolved in the 80ml deionized water, and the hydrochloric acid that adds 2mol/L is regulated about its pH value to 0.2, nano level ferric oxide particles is joined in the solution of above-mentioned zirconium oxychloride ultra-sonic dispersion 15 minutes.Above-mentioned homogeneous dispersion is tied up under the environment of 75 ℃ of heating in water bath, with magnetic agitation 6 hours.After finishing, above-mentioned dispersion system through 8000r/min centrifugation 10 minutes, is removed supernatant liquid, behind distilled water wash 2 times, oven dry obtains the particle that zirconium white out-phase coats in 60 ℃ of vacuum drying ovens.
At first prepare the aqueous solution of zirconium oxychloride: get eight hydration zirconium oxychloride (ZrOCl
28H
2O) 0.32g is dissolved in the 60ml deionized water, and it is 0.4 that the hydrochloric acid that adds 1mol/L is regulated its pH value, nano level ferric oxide particles is joined in the solution of above-mentioned zirconium oxychloride ultra-sonic dispersion 5 minutes.Above-mentioned homogeneous dispersion is tied up under the environment of 70 ℃ of heating in water bath, with magnetic agitation 24 hours.After finishing, above-mentioned dispersion system through 8000r/min centrifugation 10 minutes, is removed supernatant liquid, behind distilled water wash 3 times, oven dry obtains the particle that zirconium white out-phase coats in 60 ℃ of vacuum drying ovens.
Claims (3)
1, the preparation method of zircite cladding iron oxide powder comprises the steps:
(1) zirconium saline solution of configuration deposition precursor body, the concentration of zirconium saline solution is 0.1mmol/L～1.0mmol/L, the scope of the pH value of regulator solution is 0～2;
(2) ferric oxide particles is joined in the solution of above-mentioned zirconates, ultra-sonic dispersion 5～30 minutes,
(3) with the dispersion system of above-mentioned steps (2) gained under the environment of heating in water bath, continue to stir heating in water bath 5 minutes～48 hours;
(4) products therefrom is removed supernatant liquid through separating, and washing, dispersion and repeat number are inferior;
(5) with above-mentioned product at 15～200 ℃ of vacuum dryings, obtain zircite cladding iron oxide powder.
2, by the preparation method of the described zircite cladding iron oxide powder of claim 1, it is characterized in that the zirconates of selecting for use is Zircosol ZN, zirconium chloride, zirconium nitrate, zirconium oxychloride.
3,, it is characterized in that the grain diameter of the ferric oxide selected for use is 10nm～5 μ m by the preparation method of claim 1 or 2 described zircite cladding iron oxide powders.
4 preparation methods by claim 1 or 2 described zircite cladding iron oxide powders is characterized in that bath temperature is 15～100 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008100388238A CN101302361B (en) | 2008-06-12 | 2008-06-12 | Preparation of zircite cladding iron oxide powder |
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| CN2008100388238A CN101302361B (en) | 2008-06-12 | 2008-06-12 | Preparation of zircite cladding iron oxide powder |
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| CN101302361A true CN101302361A (en) | 2008-11-12 |
| CN101302361B CN101302361B (en) | 2011-12-14 |
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| CN2008100388238A Expired - Fee Related CN101302361B (en) | 2008-06-12 | 2008-06-12 | Preparation of zircite cladding iron oxide powder |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101707134B (en) * | 2009-11-02 | 2011-08-31 | 浙江大学 | Preparation method of high-temperature resistant superparamagnetic tin dioxide coated iron oxide nano materials |
| WO2013171044A1 (en) * | 2012-05-15 | 2013-11-21 | Siemens Aktiengesellschaft | Method for producing a storage structure of an electrical energy storage cell |
| CN108574129A (en) * | 2017-03-09 | 2018-09-25 | 天津大学 | A kind of high temperature resistant calcining iron oxide nanotube electrode and its preparation method and application |
| CN108889941A (en) * | 2018-08-01 | 2018-11-27 | 中铁四局集团第二工程有限公司 | A method of zirconium oxide is coated on tungsten carbide-cobalt composite powder body surface |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4682290B2 (en) * | 2003-02-18 | 2011-05-11 | 国立大学法人東京工業大学 | Polymer-coated metal oxide and method for producing the same |
| CN100503714C (en) * | 2006-07-28 | 2009-06-24 | 中国科学院理化技术研究所 | Method for preparing monodisperse polystyrene/zirconia core-shell glue composite ball particle |
-
2008
- 2008-06-12 CN CN2008100388238A patent/CN101302361B/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101707134B (en) * | 2009-11-02 | 2011-08-31 | 浙江大学 | Preparation method of high-temperature resistant superparamagnetic tin dioxide coated iron oxide nano materials |
| WO2013171044A1 (en) * | 2012-05-15 | 2013-11-21 | Siemens Aktiengesellschaft | Method for producing a storage structure of an electrical energy storage cell |
| CN104302425A (en) * | 2012-05-15 | 2015-01-21 | 西门子公司 | Method for producing a storage structure of an electrical energy storage cell |
| US9299979B2 (en) | 2012-05-15 | 2016-03-29 | Siemens Aktiengesellschaft | Method for producing a storage structure of an electrical energy storage cell |
| CN104302425B (en) * | 2012-05-15 | 2016-08-24 | 西门子公司 | For the method manufacturing the storage organization of energy storage unit |
| CN108574129A (en) * | 2017-03-09 | 2018-09-25 | 天津大学 | A kind of high temperature resistant calcining iron oxide nanotube electrode and its preparation method and application |
| CN108889941A (en) * | 2018-08-01 | 2018-11-27 | 中铁四局集团第二工程有限公司 | A method of zirconium oxide is coated on tungsten carbide-cobalt composite powder body surface |
| CN108889941B (en) * | 2018-08-01 | 2020-10-27 | 中铁四局集团第二工程有限公司 | Method for coating zirconium oxide on surface of tungsten carbide-cobalt composite powder |
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| CN101302361B (en) | 2011-12-14 |
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