CN101289228A - Method for preparing porous zinc ferrite nano-rods - Google Patents
Method for preparing porous zinc ferrite nano-rods Download PDFInfo
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- CN101289228A CN101289228A CNA2008100621694A CN200810062169A CN101289228A CN 101289228 A CN101289228 A CN 101289228A CN A2008100621694 A CNA2008100621694 A CN A2008100621694A CN 200810062169 A CN200810062169 A CN 200810062169A CN 101289228 A CN101289228 A CN 101289228A
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Abstract
The invention discloses a preparation method of a nano-rod of porous zinc ferrite. The preparation method adopts a four-component micro emulsion system comprising hexadecyl trimethyl bromide/water/cyclohexane/n-amyl alcohol, dissoluble zinc salt, dissoluble ferrite and oxalic acid as reactants to firstly synthesize the ZnFe2(C2O4)3 precursor of nano-rod, and then is calcined at the temperature of 500 DEG C to 900 DEG C, the nano-rod of the porous zinc ferrite, the chemical formula of which is ZnFe2O4, is obtained owing to the separation of oxalic acid radical from the precursor in the process of calcination. The nano-rod of the porous zinc ferrite is provided with a plurality of nano-pores, the products obtained by the preparation method is uniformly dispersed with good crystallization, diameter being 30nm to100nm and length being 1mum to 10mum.
Description
Technical field
The present invention relates to a kind of preparation method of porous zinc ferrite nano-rods.
Background technology
The zinc ferrite chemical formula is ZnFe
2O
4, be iron zinc binary oxide, belong to spinel structure.Use because of it has in fields such as information storage, electron device, photoconductive material and susceptible device susceptores widely, and receive much concern.Closely during the last ten years, along with the rise of nanometer technology, the research of zinc ferrite nano material and application are hot issues.Since people such as Chu have reported the zinc ferrite nano particle ethanol had very strong gas-sensitive property (X.F.Chu et al., Sens.Actuators B., 55,19 (1999)) since, people find that successively the zinc ferrite nano material all shows gas-sensitive property to numerous reducing gas such as hydrogen sulfide, carbon monoxide and ethanol.Also the reported for work zinc ferrous acid nanocrystalline body that adopts the thermal decomposition method preparation of people such as Yao at room temperature shows the character of superparamagnetism in addition, and can change its magnetic property (C.Yao et al. by the granular size that changes this magneticsubstance, J.Phys.Chem.C., 111,12274 (2007)).
Compare with nano particle, the one dimension Nano structure such as nanometer rod is because its transmission to electronics and exciton more effective (J.Polleux et al., Angew.Chem.Int.Ed., 45,261 (2006)), be more suitable for being used for nano-device, as the nanometer gas sensitive device.And, to compare with common one dimension Nano structure, the one dimension porous zinc ferrite nano-rods has bigger specific surface area and Geng Duo gaseous diffusion pipeline, and therefore, the porous nano rod is the optimal material of nanometer gas sensitive device.
At present, the investigator has adopted several different methods to prepare the zinc ferrite nano material, comprises sol-gel method, hydrothermal method, template thermal decomposition method etc., and what adopt that these methods obtain more mainly is nano particle and nanometer rod.Up to the present, there is not the people openly to report the preparation of one dimension zinc ferrite porous nanometer structure as yet.
Summary of the invention
Because conventional method prepares relatively difficulty of porous nanometer structure, the object of the present invention is to provide a kind of employing microemulsion method to prepare porous zinc ferrite nano-rods.
The technical solution used in the present invention concrete steps are as follows:
1) cetyltrimethylammonium base, n-amyl alcohol, the cyclohexane with different mol ratio is dissolved in the deionized water, and cetyltrimethylammonium base concentration is 0.02～0.08 mol/L in the control microemulsion system; Deionized water and cetyltrimethylammonium base mol ratio are 10～30; N-amyl alcohol and cetyltrimethylammonium base mol ratio are 4～8.Stir;
2) add oxalic acid solution, soluble zinc salt and soluble ferrite respectively in above-mentioned microemulsion, control oxalic acid and soluble zinc salt mol ratio are 10～50, and soluble zinc salt and soluble ferrite mol ratio are 1: 2, stir 2～24 hours;
3) product obtains ZnFe through centrifugal, drying after processing
2(C
2O
4)
3The nanometer rods presoma;
4) step 3) gained presoma was calcined 0.5～48 hour down at 500～900 ℃, promptly obtained porous zinc ferrite nano-rods.
Described soluble zinc salt is zinc nitrate Zn (NO
3)
2, zinc sulfate ZnSO
4Perhaps zinc chloride ZnCl
2
Described soluble ferrite is frerrous chloride FeCl
2Perhaps ferrous sulfate FeSO
4
Described porous zinc ferrite nano-rods, chemical formula are ZnFe
2O
4, diameter is 30～90 nanometers, length is 1～10 micron.
The beneficial effect that the present invention has is:
The present invention adopts microemulsion method, has at first prepared ZnFe
2(C
2O
4)
3The nanometer rods presoma, again with presoma 500～900 ℃ of lower calcinings since the calcination process oxalate with the separating of presoma, caused the nanostructured of porous.Therefore, products therefrom is pure zinc ferrite nano stick.Be covered with nano aperture on the nanometer rod of the present invention preparation, and product is uniformly dispersed, the well-crystallized, diameter is 30～100 nanometers, length is 1～10 micron.
Description of drawings
Fig. 1 is the XRD figure spectrum of embodiment 1 gained porous zinc ferrite nano-rods.
Fig. 2 is the field emission scanning electron microscope photo of embodiment 2 gained porous zinc ferrite nano-rods.
Fig. 3 is embodiment 3 gained porous zinc ferrite nano-rods (a) transmission electron microscope photos, (b) high-resolution-ration transmission electric-lens photo.
Embodiment
Embodiment 1:
At first cetyltrimethylammonium base, 24.145 gram (0.287 mole) hexanaphthenes and 0.846 gram (9.6 mmole) Pentyl alcohol with 0.583 gram (1.6 mmole) is dissolved in 48 ml deionized water, obtains microemulsion system after the stirring.Wherein, the cetyl trimethyl molar concentration is 0.02 mol/L, and deionized water and cetyltrimethylammonium base mol ratio are 30, and n-amyl alcohol and cetyltrimethylammonium base mol ratio are 8.The solution of ferrous chloride that the zinc nitrate solution that the oxalic acid that is 0.2 mol/L with 8 milliliters of molar concentrations respectively then, 8 milliliters of molar concentrations are 0.02 mol/L and 16 milliliters of molar concentrations are 0.02 mol/L is poured in the above microemulsion, be that oxalic acid and zinc salt mol ratio in the microemulsion is 10, zinc salt and ferrous salt mol ratio are 1: 2.Stirred 2 hours.By obtaining ZnFe after centrifugal, the dry processing
2(C
2O
4)
3The nanometer rods precursor.At last, precursor calcining under 500 ℃ was obtained porous zinc ferrite nano-rods in 48 hours.Fig. 1 is the XRD collection of illustrative plates of this porous zinc ferrite nano-rods, and this collection of illustrative plates and zinc ferrite standard card JCPDS no.22-1012 match, and do not have ZnO, Fe
2O
3Deng the diffraction maximum of impurity, illustrate that product is pure zinc ferrite, chemical formula is ZnFe
2O
4Transmission electron microscope observing shows that product is the one dimension porous nanometer structure, single nanometer rod diameter 30 nanometers, and length is 1 micron.
Embodiment 2:
At first cetyltrimethylammonium base, 8.138 gram (96.7 mmole) hexanaphthenes and 1.269 gram (14.4 mmole) Pentyl alcohols with 0.875 gram (2.4 mmole) are dissolved in 48 ml deionized water, obtain microemulsion system after the stirring.Wherein, the cetyl trimethyl molar concentration is 0.04 mol/L, and deionized water and cetyltrimethylammonium base mol ratio are 20, and n-amyl alcohol and cetyltrimethylammonium base mol ratio are 6.The copperas solution that the solution of zinc sulfate that the oxalic acid that is 0.4 mol/L with 6 milliliters of molar concentrations respectively then, 2 milliliters of molar concentrations are 0.04 mol/L and 4 milliliters of molar concentrations are 0.04 mol/L is poured in the above microemulsion, be that oxalic acid and zinc salt mol ratio in the microemulsion is 30, zinc salt and ferrous salt mol ratio are 1: 2.Stirred 10 hours.By obtaining ZnFe after centrifugal, the dry processing
2(C
2O
4)
3The nanometer rods precursor.At last, precursor calcining under 700 ℃ was obtained porous zinc ferrite nano-rods in 24 hours.By showing that the XRD collection of illustrative plates of this product and zinc ferrite standard card JCPDS no.22-1012 match, and do not have ZnO, Fe after the X-ray diffractometer test
2O
3Deng the diffraction maximum of impurity, illustrate that product is pure zinc ferrite, chemical formula is ZnFe
2O
4Fig. 2 is the field emission scanning electron microscope photo of this porous zinc ferrite nano-rods, and therefrom can obtain this product is the one dimension porous nanometer structure, and single nanometer rod diameter is 80 nanometers, and length is 10 microns.
Embodiment 3:
At first cetyltrimethylammonium base, 4.611 gram (54.78 mmole) hexanaphthenes and 1.692 gram (19.2 mmole) Pentyl alcohols with 1.166 grams (3.2 mmole) are dissolved in 32 ml deionized water, obtain microemulsion system after the stirring.Wherein, the cetyl trimethyl molar concentration is 0.08 mol/L, and deionized water and cetyltrimethylammonium base mol ratio are 10, and n-amyl alcohol and cetyltrimethylammonium base mol ratio are 4.The copperas solution that the liquor zinci chloridi that the oxalic acid that is 0.8 mol/L with 4 milliliters of molar concentrations respectively then, 6.4 milliliters of molar concentrations are 0.01 mol/L and 12.8 milliliters of molar concentrations are 0.01 mol/L is poured in the above microemulsion, be that oxalic acid and zinc salt mol ratio in the microemulsion is 50, zinc salt and ferrous salt mol ratio are 1: 2.Stirred 24 hours.By obtaining ZnFe after centrifugal, the dry processing
2(C
2O
4)
3The nanometer rods precursor.At last, precursor calcining under 900 ℃ was obtained porous zinc ferrite nano-rods in 0.5 hour.By showing that the XRD collection of illustrative plates of this product and zinc ferrite standard card JCPDS no.22-1012 match, and do not have ZnO, Fe after the X-ray diffractometer test
2O
3Deng the diffraction maximum of impurity, illustrate that product is pure zinc ferrite, chemical formula is ZnFe
2O
4Fig. 3 (a) is the transmission electron microscope photo of this porous zinc ferrite nano-rods, and therefrom can obtain this product is the one dimension porous nanometer structure, and single nanometer rod diameter is 100 nanometers, and length is 5 microns.Fig. 3 (b) is the high-resolution-ration transmission electric-lens photo of this porous zinc ferrite, and photo shows this porous nano rod well-crystallized, and spacing is 0.49nm, matches with (111) spacing of zinc ferrite.
Claims (4)
1, a kind of preparation method of porous zinc ferrite nano-rods is characterized in that the step of this method is as follows:
1) cetyltrimethylammonium base, n-amyl alcohol, the cyclohexane with different mol ratio is dissolved in the deionized water, and cetyltrimethylammonium base concentration is 0.02～0.08 mol/L in the control microemulsion system; Deionized water and cetyltrimethylammonium base mol ratio are 10～30; N-amyl alcohol and cetyltrimethylammonium base mol ratio are 4～8.Stir;
2) add oxalic acid solution, soluble zinc salt and soluble ferrite respectively in above-mentioned microemulsion, control oxalic acid and soluble zinc salt mol ratio are 10～50, and soluble zinc salt and soluble ferrite mol ratio are 1: 2, stir 2～24 hours;
3) product obtains ZnFe through centrifugal, drying after processing
2(C
2O
4)
3The nanometer rods presoma;
4) step 3) gained presoma was calcined 0.5～48 hour down at 500～900 ℃, promptly obtained porous zinc ferrite nano-rods.
2, the preparation method of a kind of porous zinc ferrite nano-rods according to claim 1 is characterized in that: described soluble zinc salt is zinc nitrate Zn (NO
3)
2, zinc sulfate ZnSO
4Perhaps zinc chloride ZnCl
2
3, the preparation method of a kind of porous zinc ferrite nano-rods according to claim 1 is characterized in that: described soluble ferrite is frerrous chloride FeCl
2Perhaps ferrous sulfate FeSO
4
4, the preparation method of a kind of porous zinc ferrite nano-rods according to claim 1 is characterized in that: described porous zinc ferrite nano-rods, chemical formula are ZnFe
2O
4, diameter is 30～90 nanometers, length is 1～10 micron.
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Cited By (13)
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|---|---|---|---|---|
| CN101871122A (en) * | 2010-06-10 | 2010-10-27 | 同济大学 | Preparation method of Pt-endpoint FeNi nano rod |
| CN101508468B (en) * | 2009-04-03 | 2010-12-08 | 华中师范大学 | Nano-superstructure polyporous material of ferrite and method of preparing the same |
| CN102280634A (en) * | 2011-07-05 | 2011-12-14 | 南开大学 | Lithium manganese oxide electrode material with porous structure as well as manufacturing method and application thereof |
| CN102660770A (en) * | 2011-02-25 | 2012-09-12 | 大连理工大学 | Preparation method for ZnMn2O4 nanorod by using alpha-MnO2 nanorod template method |
| CN103435104A (en) * | 2013-06-04 | 2013-12-11 | 东莞上海大学纳米技术研究院 | Preparation method for lithium ion battery negative electrode material-nano zinc ferrite |
| CN103611536A (en) * | 2013-11-27 | 2014-03-05 | 安徽师范大学 | Pure-phase nickel ferrite nano material as well as preparation method thereof and preparation method of aromatic amine |
| CN103754953A (en) * | 2014-01-28 | 2014-04-30 | 南京信息工程大学 | Preparation method of multi-morphologynano-sized zinc ferrite |
| CN103880090A (en) * | 2014-03-26 | 2014-06-25 | 安徽师范大学 | Preparation method and application of AgFeO2 nanoparticle gas sensitive material |
| CN104085930A (en) * | 2014-06-30 | 2014-10-08 | 陕西师范大学 | Method for preparing porous flake zinc ferrite with large specific surface area |
| CN106745302A (en) * | 2017-02-27 | 2017-05-31 | 陕西科技大学 | A kind of coralloid zinc ferrite powder of three-dimensional network and preparation method thereof |
| CN109534406A (en) * | 2018-11-21 | 2019-03-29 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of electrode material ferrous acid europium and products thereof and application |
| CN110639529A (en) * | 2019-09-12 | 2020-01-03 | 中国科学院高能物理研究所 | Catalyst for removing hexavalent uranium through visible light catalytic reduction, method and application |
| CN111153438A (en) * | 2020-01-03 | 2020-05-15 | 济南大学 | ZnMn2O4 hollow rod and preparation method and application thereof |
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2008
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101508468B (en) * | 2009-04-03 | 2010-12-08 | 华中师范大学 | Nano-superstructure polyporous material of ferrite and method of preparing the same |
| CN101871122A (en) * | 2010-06-10 | 2010-10-27 | 同济大学 | Preparation method of Pt-endpoint FeNi nano rod |
| CN101871122B (en) * | 2010-06-10 | 2012-05-23 | 同济大学 | Preparation method of Pt-endpoint FeNi nano rod |
| CN102660770A (en) * | 2011-02-25 | 2012-09-12 | 大连理工大学 | Preparation method for ZnMn2O4 nanorod by using alpha-MnO2 nanorod template method |
| CN102280634A (en) * | 2011-07-05 | 2011-12-14 | 南开大学 | Lithium manganese oxide electrode material with porous structure as well as manufacturing method and application thereof |
| CN102280634B (en) * | 2011-07-05 | 2013-04-10 | 南开大学 | Lithium manganese oxide electrode material with porous structure as well as manufacturing method and application thereof |
| CN103435104A (en) * | 2013-06-04 | 2013-12-11 | 东莞上海大学纳米技术研究院 | Preparation method for lithium ion battery negative electrode material-nano zinc ferrite |
| CN103435104B (en) * | 2013-06-04 | 2015-08-19 | 东莞上海大学纳米技术研究院 | A kind of preparation method of lithium ion battery negative electrode material-nano zinc ferrite |
| CN103611536A (en) * | 2013-11-27 | 2014-03-05 | 安徽师范大学 | Pure-phase nickel ferrite nano material as well as preparation method thereof and preparation method of aromatic amine |
| CN103611536B (en) * | 2013-11-27 | 2015-09-23 | 安徽师范大学 | The preparation method of a kind of pure phase nickel ferrite based magnetic loaded nano material and preparation method thereof, a kind of arylamine |
| CN103754953A (en) * | 2014-01-28 | 2014-04-30 | 南京信息工程大学 | Preparation method of multi-morphologynano-sized zinc ferrite |
| CN103754953B (en) * | 2014-01-28 | 2015-07-22 | 南京信息工程大学 | Preparation method of multi-morphologynano-sized zinc ferrite |
| CN103880090A (en) * | 2014-03-26 | 2014-06-25 | 安徽师范大学 | Preparation method and application of AgFeO2 nanoparticle gas sensitive material |
| CN103880090B (en) * | 2014-03-26 | 2015-07-22 | 安徽师范大学 | Preparation method and application of AgFeO2 nanoparticle gas sensitive material |
| CN104085930A (en) * | 2014-06-30 | 2014-10-08 | 陕西师范大学 | Method for preparing porous flake zinc ferrite with large specific surface area |
| CN104085930B (en) * | 2014-06-30 | 2015-11-18 | 陕西师范大学 | A kind of preparation method of bigger serface porous flake zinc ferrite |
| CN106745302A (en) * | 2017-02-27 | 2017-05-31 | 陕西科技大学 | A kind of coralloid zinc ferrite powder of three-dimensional network and preparation method thereof |
| CN109534406A (en) * | 2018-11-21 | 2019-03-29 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of electrode material ferrous acid europium and products thereof and application |
| CN110639529A (en) * | 2019-09-12 | 2020-01-03 | 中国科学院高能物理研究所 | Catalyst for removing hexavalent uranium through visible light catalytic reduction, method and application |
| CN111153438A (en) * | 2020-01-03 | 2020-05-15 | 济南大学 | ZnMn2O4 hollow rod and preparation method and application thereof |
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