CN1245777A - Preparation method of zinc oxide microparticles with specific form - Google Patents
Preparation method of zinc oxide microparticles with specific form Download PDFInfo
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- CN1245777A CN1245777A CN 99117072 CN99117072A CN1245777A CN 1245777 A CN1245777 A CN 1245777A CN 99117072 CN99117072 CN 99117072 CN 99117072 A CN99117072 A CN 99117072A CN 1245777 A CN1245777 A CN 1245777A
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- Prior art keywords
- tensio
- active agent
- zinc oxide
- zinc
- preparation
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 19
- 239000011859 microparticle Substances 0.000 title claims description 9
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 239000004094 surface-active agent Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims abstract description 4
- 229920000053 polysorbate 80 Polymers 0.000 claims abstract description 4
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 18
- 239000013543 active substance Substances 0.000 claims description 17
- DKPFZGUDAPQIHT-UHFFFAOYSA-N butyl acetate Chemical compound CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 16
- 239000004246 zinc acetate Substances 0.000 claims description 15
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 14
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 12
- -1 polyoxyethylene Polymers 0.000 claims description 10
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 238000005119 centrifugation Methods 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- 239000007795 chemical reaction product Substances 0.000 claims description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 3
- 150000003752 zinc compounds Chemical class 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 239000007853 buffer solution Substances 0.000 claims description 2
- OAIYNRAQCIOEBD-UHFFFAOYSA-N butyl acetate;hydrate Chemical compound O.CCCCOC(C)=O OAIYNRAQCIOEBD-UHFFFAOYSA-N 0.000 claims description 2
- 238000000593 microemulsion method Methods 0.000 claims description 2
- 239000003637 basic solution Substances 0.000 claims 2
- 239000002245 particle Substances 0.000 abstract description 11
- 239000000376 reactant Substances 0.000 abstract description 5
- 239000012046 mixed solvent Substances 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 abstract description 2
- 125000000524 functional group Chemical group 0.000 abstract description 2
- 230000002209 hydrophobic effect Effects 0.000 abstract description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 abstract 2
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical class OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 abstract 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 abstract 1
- 239000003960 organic solvent Substances 0.000 abstract 1
- 229940068918 polyethylene glycol 400 Drugs 0.000 abstract 1
- 239000004530 micro-emulsion Substances 0.000 description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 10
- 230000000694 effects Effects 0.000 description 7
- 235000019270 ammonium chloride Nutrition 0.000 description 5
- 239000002105 nanoparticle Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000000693 micelle Substances 0.000 description 2
- 230000010355 oscillation Effects 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000009283 thermal hydrolysis Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- IPCXNCATNBAPKW-UHFFFAOYSA-N zinc;hydrate Chemical compound O.[Zn] IPCXNCATNBAPKW-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention provides a preparation method of zinc oxide ultramicro particles with different special forms. It is characterized by that said invention selects the non-ionic small-molecular surfactants (such as dehydrated sorbite, oxirene ether, monooleate, tween-80) with lipophilic/hydrophilic (HLB) chain segment ratio (less than or equal to 8), functional group, molecular weight and surface charging property, and selects the non-ionic macromolecular surfactant with specific polymerization range and polarity, for example polyethylene glycol 400, and in the set water, surfactants and hydrophobic organic solvent or its mixed solvent system and under the actions of specific temp., concentration, pH value, ultrasonic frequency and power condition it can form microreactor with specific size and form, then makes the reactant dissolve or solubilize and disperse in it and controls its chemical reaction and crystal growth to obtain the various nanometer and submicron zinc oxide particles with spherical, quasi-spherical, rod, needle and other forms.
Description
The invention belongs to the preparation method of zinc oxide microparticles.
Size of particles, form and structure and accumulation process thereof and aggregated structure have very important meaning to giving of material property, therefore since nineteen ninety-two to synthesize Jie's sight and even micron, nanoscale with chemical process, the inorganic materials with complicated form becomes very noticeable.Zinc has special role to body immunity and life-span.Special semiconduction, piezoelectricity, fluorescence, ultraviolet absorption and the shielding that ultra micro, particularly nano zine oxide had, non-linear optical performance, catalytic performance etc. are especially paid close attention to for people.Usually the resulting zinc oxide of preparation is that the sphere of six sides, single shaft crystallographic system or torispherical particle, particle diameter are also bigger.Control thermal hydrolysis and microemulsion (reverse micelle) method can make ball shaped nano zinc oxide particle.In the nano structural material preparation field, microemulsion method is a kind of method relatively more commonly used, be as microreactor mostly with water-in-oil (w/o) type microemulsion or reverse micelle, reactant reacts the generation solid phase therein, because processes such as nucleation, growth, coalescent, reunion are subjected to the restriction of microreactor, thereby form the nanoparticle that is enclosed with the layer of surface promoting agent and has certain aggregated structure and form, also avoided interparticle reunion simultaneously.Surfactant structure and character decisive role always in the whole process of film micro area prepared in reaction nano material, to can form microreactor and form after structure, form all important influence of microreactor interface film strength, reactant molecule seeing through on interfacial film, transmission and absorption property.Present used tensio-active agent mostly is small organic molecule, and applicable system is also more single, in the nano composite material of preparation different shape certain restriction is arranged.(the Guangzhou chemistry, the third phase, P37-41)
The objective of the invention is to utilize tensio-active agent with ad hoc structure and the superpolymer that can be used as tensio-active agent, and mouse out the mixed solvent system that is suitable for it, find out microreactor that forms specific size and form and the conditions suitable that reacts, order reaction and crystal (particle) control growing in formed microreactor, the zinc oxide microparticles that has specific size, form and structure with preparation.
Implementation method key of the present invention is to select for use to have specific oleophylic/the organic molecule tensio-active agent of hydrophilic (HLB) segment ratio, functional group, molecular weight and chargeding performance, with specific aggregation degree scope, polarity, non-ionic type polymer as polymeric surface active agent, with zinc salt (as zinc acetate), organic zinc compounds/water-tensio-active agent/hydrophobic organic compound or its mixed solvent system, disperse under the what design temperature, in the ultrasonic wave of CF and power and the reaction certain hour, can make the zinc oxide microparticles of stable specific form.Concrete steps with the preparation of specific form zinc oxide microparticles comprise:
0.1-0.5mol/l zinc acetate or organic zinc acetate compound and the pH value ammoniacal liquor/chloride buffer solution for 8-13 is joined in tensio-active agent/dispersion solvent system mixing solutions, form two microemulsion systems down in the ultrasonic wave effect at a certain temperature, in frequency is 25KHz, power is reaction 2-3 hour in the ultrasound reactor of 400W, product obtains to be enclosed with the nano zine oxide of tensio-active agent through 3000 rev/mins of centrifugations.The tensio-active agent that uses is the tween-80 of HLB value as 7-8, W=6-20, water/hexanaphthene of temperature of reaction 28-40 ℃ (volume ratio 1: 30-50) mixed solvent system, reactant concn 0.5-1mol/l, when surfactant concentration is 4.5-7.0g/L, 7.0-10.0g/L, 10.0-16g/L, can make sphere, bar-shaped and sheet zinc oxide nanoparticle respectively; Tensio-active agent is the polyoxyethylene glycol of polymerization degree 200-400, W=6-20, in water/N-BUTYL ACETATE of temperature of reaction 35-46 ℃/hexanaphthene (volume ratio 1: 50: 30) mixed solution system, reactant concn is 0.1-0.5mol/l, surfactant concentration is 8-20g/L, can make respectively have sphere, needle-like, hexagonal plate, bar-shaped, zinc oxide microparticles that spiral is bar-shaped.
Preparation method of the present invention, except that can obtain to have sphere, the torispherical nano zine oxide, can also make the nano zinc oxide particles of bar-shaped, needle-like, lumen shape, hexagonal plate, can also obtain length and have spiral, double-stranded nanometer, the bar-shaped zinc oxide microparticles of submicron more than 15 microns.
Embodiment 1: with 0.5-1mol/L zinc acetate solution or sodium hydroxide solution, 7.0-12g/L Span-80 (water/tensio-active agent is than W=6-8) and hexanaphthene add in the reactor successively, disperseed 45 minutes at 32 ℃ of following sonic oscillations, resulting zinc acetate and sodium hydroxide microemulsion are mixed, reaction is 1-1.5 hour under the ultrasonic oscillation condition, make the microemulsion that contains bar-shaped zinc oxide nano-particle, wherein the diameter of nanoparticle is 20-30nm, length-to-diameter ratio 〉=20.
Embodiment 2: with 0.5-1mol/L zinc acetate or sodium hydroxide solution, the Span-80 of 15-18g/L (W=10-18) and hexanaphthene add in the reactor successively, shake dispersion 45-60 minute down at 25-28 ℃, prepared zinc acetate and sodium hydroxide microemulsion are mixed, what 25-28 ℃ was reacted 1-2 hour under ultrasound condition, made the microemulsion of the nano zinc oxide particles that contains single chamber and multi-cavity lumen shape aggregated structure (the about 20-30nm of each independent dispersed particle particle dia that forms cavity).
Embodiment 3: the ammoniacal liquor/ammonium chloride solution 0.1-0.5mL for 8-13 joins respectively in 0.2-0.6mL polyoxyethylene glycol-400/4-16mL N-BUTYL ACETATE/4-16mL hexanaphthene mixing solutions with the 1mol/L zinc acetate of 0.1-0.5mL and pH value, constant temperature in 37-46 ℃, under the ultrasonic wave effect, disperseed 1 hour, after forming two microemulsion systems, two microemulsion systems are mixed, under 37-46 ℃, continuation was reacted in ultrasonic wave 2 hours, the reaction product that obtains obtains flaky nanometer zinc oxide 3000 rev/mins of following centrifugations.
Embodiment 4: the ammoniacal liquor/ammonium chloride solution 0.05-0.25mL for 8-13 joins respectively in 0.2-0.6mL polyoxyethylene glycol-200/6-18mL N-BUTYL ACETATE/6-18mL hexanaphthene mixing solutions with the 1mol/L zinc acetate of 0.1-0.5mL and pH value, constant temperature in 35-46 ℃, under the ultrasonic wave effect, disperseed 1 hour, after forming two microemulsion systems, two microemulsion systems are mixed, under 44 ℃, continuation was reacted in ultrasonic wave 2 hours, the reaction product that obtains obtains even spherical nano zine oxide 3000 rev/mins of following centrifugations.
Embodiment 5: the ammoniacal liquor/ammonium chloride solution 0.6-1.0mL for 8-12 joins respectively in 0.2-0.6mL polyoxyethylene glycol-400/8-12mL N-BUTYL ACETATE/6-10mL hexanaphthene mixing solutions with the 1mol/L zinc acetate of 0.25-0.6mL and pH value, constant temperature in 46 ℃, under the ultrasonic wave effect, disperseed 1 hour, after forming two microemulsion systems, two microemulsion systems are mixed, under 44 ℃, continuation was reacted in ultrasonic wave 2 hours, the reaction product that obtains obtains duplex shape nano zine oxide 3000 rev/mins of following centrifugations.
Embodiment 6: the sodium hydroxide solution 0.1-0.3mL for 11-13 joins respectively in 0.2-0.4mL polyoxyethylene glycol-400/8-12mL N-BUTYL ACETATE/6-10mL hexanaphthene mixing solutions with the 1mol/L zinc acetate of 0.1-0.4mL and pH value, constant temperature in 44 ℃, under the ultrasonic wave effect, disperseed 1 hour, after forming two microemulsion systems, two microemulsion systems are mixed, under 44 ℃, continuation was reacted in ultrasonic wave 2 hours, the reaction product that obtains obtains needle-shape nano zinc oxide 3000 rev/mins of following centrifugations.
Embodiment 7: the ammoniacal liquor/ammonium chloride solution 0.25-0.6mL for 8-12 joins respectively in 0.2-0.5mL polyoxyethylene glycol-200/4.0-8.0mL N-BUTYL ACETATE/8-12mL hexanaphthene mixing solutions with the 1mol/L zinc acetate of 0.1-0.4mL and pH value, constant temperature in 44 ℃, under the ultrasonic wave effect, disperseed 1 hour, after forming two microemulsion systems, two microemulsion systems are mixed, under 44 ℃, continuation was reacted in ultrasonic wave 2 hours, the reaction product that obtains obtains the spirrillum nano zine oxide 3000 rev/mins of following centrifugations.
Embodiment 8: the ammoniacal liquor/ammonium chloride solution 0.3-0.8mL for 8-12 joins respectively in 0.25-0.5mL polyoxyethylene glycol-200/3.0-8.0mL N-BUTYL ACETATE/8-14mL hexanaphthene mixing solutions with the 1mol/L zinc acetate of 0.05-0.25mL and pH value, constant temperature in 44 ℃, under the ultrasonic wave effect, disperseed 1 hour, after forming two microemulsion systems, two microemulsion systems are mixed, under 44 ℃, continuation was reacted in ultrasonic wave 2 hours, the reaction product that obtains obtains the hexagonal plate nano zine oxide 3000 rev/mins of following centrifugations.
Claims (3)
1. one kind prepares the method with specific form zinc oxide microparticles.This method is ultrasonic microemulsion method, it is characterized in that adopting tween-80 or polyoxyethylene glycol (PEG) is tensio-active agent, zinc acetate or organic zinc compound and basic solution are joined respectively in tensio-active agent/dispersion solvent mixing solutions, in frequency is 25KHz, power is to react in the ultrasound reactor of 400W, reaction product obtains to be enclosed with the nano zine oxide of tensio-active agent through centrifugation.
2. according to claims 1 described method, it is characterized in that can being following form when employed tensio-active agent/dispersion solvent mixing solutions:
When (1) tensio-active agent was tween-80, the HLB value was about 7-8, W=6-20, temperature of reaction 28-
40 ℃, water/hexanaphthene volume proportion is 1: 30-50, surfactant concentration is respectively 4.5-
7.0g/L、7.0-10.0g/L、10.0-16g/L。
(2) tensio-active agent is the polyoxyethylene glycol (PEG) of polymerization degree 200-400, W=6-20, reaction temperature
Water/N-BUTYL ACETATE/hexanaphthene the volume proportion of spending 35-46 ℃ is 1: 50: 30, tensio-active agent
Concentration is 8-20g/L.
3. according to claims 1 described method, it is characterized in that described zinc acetate or organic zinc compound concentration are 0.1-0.5mol/l, described basic solution is ammoniacal liquor/chloride buffer solution of pH8-13.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99117072A CN1079080C (en) | 1999-09-08 | 1999-09-08 | Preparation method of zinc oxide microparticles with specific form |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99117072A CN1079080C (en) | 1999-09-08 | 1999-09-08 | Preparation method of zinc oxide microparticles with specific form |
Publications (2)
| Publication Number | Publication Date |
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| CN1245777A true CN1245777A (en) | 2000-03-01 |
| CN1079080C CN1079080C (en) | 2002-02-13 |
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| CN99117072A Expired - Fee Related CN1079080C (en) | 1999-09-08 | 1999-09-08 | Preparation method of zinc oxide microparticles with specific form |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2853307A1 (en) * | 2003-04-07 | 2004-10-08 | Centre Nat Rech Scient | Preparing uniformly shaped and sized metal oxide nanoparticles, by spontaneous oxidation of selected organometallic precursors in non-aqueous solvent |
| CN100372777C (en) * | 2006-01-19 | 2008-03-05 | 浙江大学 | Method for preparing different shaped nano zinc oxide by thermal decomposition |
| CN100460334C (en) * | 2007-02-25 | 2009-02-11 | 华中师范大学 | Preparation of graduated nano-structural transition metal oxide by two-phase solvent soft interface process |
| CN101475206B (en) * | 2009-01-13 | 2010-06-02 | 东华大学 | Method for preparing ZnO nanorod with controllable distribution by growing in microchannel |
| CN101811727A (en) * | 2010-04-16 | 2010-08-25 | 广西民族大学 | Method for synthesizing flaky nano zinc oxide by low-temperature control |
| WO2010115320A1 (en) * | 2009-04-10 | 2010-10-14 | 北京化工大学 | Integral porous adsorbent and preparation method therefor |
| CN101235222B (en) * | 2007-12-28 | 2010-12-01 | 太仓诚信化工有限公司 | Preparation method of zinc oxide for rubber |
| CN102101693A (en) * | 2010-12-29 | 2011-06-22 | 安徽理工大学 | Preparation method and application of double-function micro-nano hierarchical structural zinc oxide power |
| CN102134091A (en) * | 2011-01-21 | 2011-07-27 | 陕西师范大学 | Method for preparing micro structural zinc oxide by hydrothermal method |
| CN107090194A (en) * | 2017-05-15 | 2017-08-25 | 广西放心源生物科技有限公司 | A kind of method of surface treating nano zinc oxide |
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| CN1295384C (en) * | 2004-06-25 | 2007-01-17 | 中国科学院广州化学研究所 | Process for collimated beam shaped nano zinc oxide crystal whisker |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0244765B2 (en) * | 1983-03-16 | 1990-10-05 | Inoue Japax Res | KINZOKUFUKUSANKABUTSUNOSEIZOHOHO |
| FR2677558B1 (en) * | 1991-06-14 | 1995-01-06 | Commissariat Energie Atomique | PROCESS AND DEVICE FOR MANUFACTURING INORGANIC ULTRAFINE POWDERS BY AEROSOL-LASER COUPLING. |
| CN1083538A (en) * | 1992-08-29 | 1994-03-09 | 中国科学院化工冶金研究所 | The preparing zinc-oxide by use of plasma method Processes and apparatus |
| CN1184079A (en) * | 1996-12-05 | 1998-06-10 | 云南大学 | Supersonic emulsifying co-precipitation process preparing compound zinc oxide voltage-sensitive resistor powder |
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1999
- 1999-09-08 CN CN99117072A patent/CN1079080C/en not_active Expired - Fee Related
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| WO2004092069A3 (en) * | 2003-04-07 | 2005-03-10 | Centre Nat Rech Scient | Method for the preparation of a composition of nanoparticles of at least one crystalline metal oxide |
| US7704413B2 (en) | 2003-04-07 | 2010-04-27 | Centre National De La Recherche Scientifique (C.N.R.S.) | Method for the preparation of a composition of nanoparticles of at least one crystalline metal oxide |
| FR2853307A1 (en) * | 2003-04-07 | 2004-10-08 | Centre Nat Rech Scient | Preparing uniformly shaped and sized metal oxide nanoparticles, by spontaneous oxidation of selected organometallic precursors in non-aqueous solvent |
| CN100372777C (en) * | 2006-01-19 | 2008-03-05 | 浙江大学 | Method for preparing different shaped nano zinc oxide by thermal decomposition |
| CN100460334C (en) * | 2007-02-25 | 2009-02-11 | 华中师范大学 | Preparation of graduated nano-structural transition metal oxide by two-phase solvent soft interface process |
| CN101235222B (en) * | 2007-12-28 | 2010-12-01 | 太仓诚信化工有限公司 | Preparation method of zinc oxide for rubber |
| CN101475206B (en) * | 2009-01-13 | 2010-06-02 | 东华大学 | Method for preparing ZnO nanorod with controllable distribution by growing in microchannel |
| WO2010115320A1 (en) * | 2009-04-10 | 2010-10-14 | 北京化工大学 | Integral porous adsorbent and preparation method therefor |
| CN101811727A (en) * | 2010-04-16 | 2010-08-25 | 广西民族大学 | Method for synthesizing flaky nano zinc oxide by low-temperature control |
| CN102101693A (en) * | 2010-12-29 | 2011-06-22 | 安徽理工大学 | Preparation method and application of double-function micro-nano hierarchical structural zinc oxide power |
| CN102134091A (en) * | 2011-01-21 | 2011-07-27 | 陕西师范大学 | Method for preparing micro structural zinc oxide by hydrothermal method |
| CN102134091B (en) * | 2011-01-21 | 2013-04-17 | 陕西师范大学 | Method for preparing micro structural zinc oxide by hydrothermal method |
| CN107090194A (en) * | 2017-05-15 | 2017-08-25 | 广西放心源生物科技有限公司 | A kind of method of surface treating nano zinc oxide |
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| CN1079080C (en) | 2002-02-13 |
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