CN103214026B - Preparation method of CaO/ZnO core-shell structure nanometer material - Google Patents
Preparation method of CaO/ZnO core-shell structure nanometer material Download PDFInfo
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- CN103214026B CN103214026B CN201310175824.8A CN201310175824A CN103214026B CN 103214026 B CN103214026 B CN 103214026B CN 201310175824 A CN201310175824 A CN 201310175824A CN 103214026 B CN103214026 B CN 103214026B
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Abstract
The invention discloses a preparation method of a CaO/ZnO core-shell structure nanometer material and belongs to the technical field of material science. The preparation method of the CaO/ZnO core-shell structure nanometer material comprises the following steps of: dispersing CaCO3 nanospheres in a mixed solution of H2O and DMF (Dimethyl Formamide), wherein the volume ratio of the H2O to the DMF is (7:3) to (8:2); adding Zn(AcO) to the mixed solution, so that the molar ratio of Zn to Ca is (5:1) to (7:1); continuously stirring and ageing at the room temperature; centrifuging to collect precipitates and drying the precipitates in vacuum; and calcining to obtain the CaO/ZnO core-shell structure nanometer material. The CaO/ZnO core-shell structure nanometer material prepared by using the preparation method disclosed by the invention is adjustable in shape and structure and higher in yield. Moreover, the preparation method is simple in process, convenient to operate and beneficial to industrialization.
Description
Technical field
The invention belongs to materialogy technical field, be specifically related to a kind of simple and convenient process for preparing of CaO/ZnO nuclear shell structured nano-material.
Background technology
Nuclear shell structured nano-material is used widely multi-field because of core core composition and the shell composition with functionalization, as susceptor, pharmaceutical carrier, biomedical imaging, catalyzer, photocatalyst (comprising fuel cell) etc., therefore such material also receives numerous investigators' concern.The method of preparing nuclear shell structured nano-material has a lot, and template has efficient, easy feature and is often used to prepare spherical nuclear shell structured nano-material.Conventional mould material has a lot, as hard template comprises silicon ball, polystyrene emulsion and soft template etc.Nanometer CaCO
3there is stronger perviousness, the aspect such as prepare at pigment, opticglass, pottery and electrical condenser and be used widely.CaCO
3microballoon can, by being decomposed to form CaO, be particularly suitable for preparing Core-Shell Particles as template, with CaCO
3the research that nanometer ball is prepared CaO/ZnO nuclear shell structured nano-material as template there is not yet report.
At present, ZnO is used widely in a lot of fields as functional type semiconductor material, as field-effect transistor, dyestuff activation solar cell, biosensor and solid phase air-sensitive probe etc.ZnO has wide potential using value, and the research of its form and distribution is paid close attention to.Wet chemistry method, spray-drying process and hot solution method or hydrothermal method are the common methods of making ZnO.Synthetic environment can affect the microstructure of ZnO as form conditioning agent and reaction medium, bibliographical information, and synthetic regular nano-ZnO, can present different structures, as bar-shaped, nano wire, star, quadrangle, flower shape, spherical and height symmetrical structure etc.But less about the research report of preparation CaO/ZnO nuclear shell structured nano-material, compared with the ZnO nano material of low dimension, CaO/ZnO nuclear shell structured nano-material has height aggregation, extinction effect and photocatalytic activity.
Invention Inner holds
The object of the present invention is to provide a kind of short-cut method of the CaO/ZnO of preparation nuclear shell structured nano-material, by CaCO
3nanometer ball is distributed to H
2in the mixed solution of O and DMF; Again by Zn (AcO)
2join in mixed solution continuously stirring; Room temperature ageing; Centrifugal collecting precipitation: vacuum-drying; By high-temperature calcination, form the CaO/ZnO nuclear shell structured nano-material of the different shapes such as spherical or class is spherical.
The present invention prepares CaO/ZnO nuclear shell structured nano-material by the precipitator method in easy liquid, and this material has core core composition CaO and shell composition ZnO.With CaCO
3nanometer ball is as template and form conditioning agent, and Zn (OH)
2layer forms by precipitation process in liquid, after high-temperature calcination, obtains CaO/ZnO nuclear shell structured nano-material.
The preparation method of CaO/ZnO nuclear shell structured nano-material:
(1) CaCO
3nanometer ball is distributed to H
2in the mixed solution of O and DMF; In mixed solution, CaCO
3concentration be 0.08～0.10mol/L, H
2the volume ratio of O and DMF is 7:3～8:2;
(2) by Zn (AcO)
2join in above-mentioned mixed solution, the mol ratio that makes Zn/Ca is 5:1～7:1, continuously stirring 10～18h;
(3) room temperature ageing 12～36h;
(4) 3000～8000rpm centrifugal collecting precipitations;
(5) the dry 12～72h of normal-temperature vacuum;
(6) 450～830 DEG C of calcining 1～3h, the nano material of formation CaO/ZnO composite structure.
Nanometer CaCO
3purchased from Shanghai reagent company.Zinc acetate (Zn (AcO)
2) and DMF (DMF) be analytical pure, when application, do not need purifying, the water using in all experiments were process is deionized water.Under normal temperature and pressure conditions, characterize by XRD, SEM and forming process, form and the structure of TEM to product.
Method provided by the invention has the following advantages and high-lighting effect compared with existing preparation method: nuclear shell structured nano-material product form and structure prepared by the method can regulate and control; Productive rate is higher; Technique is simple, easy to operate, is beneficial to industrialization.
Brief description of the drawings
The XRD spectra of CaO/ZnO nuclear shell structured nano-material prepared by Fig. 1: embodiment 1, illustrates and in prepared material, includes CaO and ZnO;
Fig. 2: CaO/ZnO nuclear shell structured nano-material TEM photo prepared by different Zn/Ca mol ratios (Fig. 2 a5:1, Fig. 2 b7:1);
Fig. 3: CaO/ZnO nuclear shell structured nano-material TEM photo prepared by differential responses temperature (Fig. 3 a450 DEG C, Fig. 3 b830 DEG C);
Fig. 4: different H
2caO/ZnO nuclear shell structured nano-material TEM photo prepared by the volume ratio (Fig. 4 a8:2, Fig. 4 b7:3) of O/DMF.
Embodiment
The CaO/ZnO nuclear shell structured nano-material with core core composition CaO and shell composition ZnO is to prepare by the precipitator method in easy liquid.By CaCO
3nanometer ball is distributed in the mixed solution of water and DMF, then zinc acetate is joined in mixed solution, continues to stir.Through high-temperature calcination, obtain CaO/ZnO nuclear shell structured nano-material.
Further illustrate preparation method and the feature thereof of CaO/ZnO nuclear shell structured nano-material of the present invention below by several exemplary embodiments.
1, the CaO/ZnO nuclear shell structured nano-material that prepared by different Zn/Ca mol ratios
Embodiment 1:
CaCO
3nanometer ball (particle diameter 60-80nm) is distributed to H
2in the mixed solution of O and DMF, then, by the Zn of difference amount (AcO)
2(calculating with Zn/Ca mol ratio) joins in this mixed solution, continues to stir ageing.Centrifugal collecting precipitation, vacuum-drying.By high-temperature calcination, form CaO/ZnO nuclear shell structured nano-material.
When Zn/Ca mol ratio is 5:1, the form of prepared CaO/ZnO nuclear shell structured nano-material is that stub shape or class are spherical, slightly assembles.Zn/Ca mol ratio is 7:1, and prepared CaO/ZnO nuclear shell structured nano-material is spherical, and particle diameter is increased to 500nm, microballoon good dispersity, and the thickness of ZnO shell is about 50nm.
2, the CaO/ZnO nuclear shell structured nano-material that prepared by different calcining temperatures
Embodiment 2:
CaCO
3nanometer ball is distributed to H
2in the mixed solution of O and DMF, by Zn (AcO)
2join in this mixed solution continuously stirring, ageing.Centrifugal collecting precipitation, vacuum-drying.By high-temperature calcination, form CaO/ZnO nuclear shell structured nano-material.At 450 DEG C, form CaO/ZnO nuclear shell structured nano-microballoon, particle diameter is 80nm, the thickness of the ZnO shell on CaO surface is about 10.0nm, when temperature of reaction is elevated to 830 DEG C, forms CaO/ZnO nuclear shell structured nano-microballoon, particle diameter is 200nm, and the thickness of the ZnO shell on CaO surface is about 10.0nm.
3, different H
2caO/ZnO nuclear shell structured nano-material prepared by the volume ratio of O/DMF
Embodiment 3:
CaCO
3nanometer ball is distributed to H
2o and DMF(different volumes ratio) mixed solution in, then, by Zn (AcO)
2join in this mixed solution continuously stirring, ageing.Centrifugal collecting precipitation, vacuum-drying.By high-temperature calcination, form CaO/ZnO nuclear shell structured nano-material.H
2when the volume ratio of O/DMF is higher, form the material (being the spherical nucleocapsid structure of stub shape or class) that is about 100 nanometers, wide about 10nm, H
2o/DMF ratio is 7:3, forms spherical nuclear shell structured nano-material, and particle diameter is about 250nm, and shell thickness is about 10.0nm.
In conjunction with specific embodiments, the present invention is done to further elaboration above, instead of will limit the invention with this.Inventive point of the present invention is to prepare CaO/ZnO nuclear shell structured nano-material by the precipitator method in easy liquid, is by CaCO
3nano material is distributed in the mixed solution of water and DMF, zinc acetate joins in mixed solution, continuously stirring, through high-temperature calcination, obtain CaO/ZnO nuclear shell structured nano-material, this material has core core composition CaO and shell composition ZnO, as for other mould materials beyond Application Example, solvent material, core core material, Shell Materials, digestion time, calcining temperature, time etc. all within the scope of design of the present invention.
Claims (1)
1. a preparation method for CaO/ZnO nuclear shell structured nano-material, its step is as follows:
(1) by CaCO
3nanometer ball is distributed to H
2in the mixed solution of O and DMF; H
2the volume ratio of O and DMF is 7:3～8:2; CaCO
3concentration be 0.08～0.10mol/L;
(2) by Zn (AcO)
2join in above-mentioned mixed solution, the mol ratio that makes Zn/Ca is 5:1～7:1, continuously stirring; The time of stirring is 10～18h;
(3) room temperature ageing; The time of room temperature ageing is 12～36h;
(4) centrifugal collecting precipitation; Centrifugal speed is 3000～8000rpm;
(5) normal-temperature vacuum is dry; The vacuum drying time is 12～72h;
(6) after calcining, obtain CaO/ZnO nuclear shell structured nano-material, the temperature of calcining is 450～830 DEG C, and the time of calcining is 1～3h.
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| CN106924052B (en) * | 2017-03-24 | 2020-08-11 | 吉林大学 | CaO nanoparticle antibacterial material with ZnO coating and preparation method thereof |
| CN109938039A (en) * | 2019-04-19 | 2019-06-28 | 泉州师范学院 | A kind of preparation method and antibacterial applications of CaO/ZnO composite nano materials |
| CN111606351B (en) * | 2020-05-21 | 2021-08-24 | 江南大学 | Zinc oxide coated calcium carbonate nano material and preparation method thereof |
| CN114436320B (en) * | 2022-01-25 | 2023-12-05 | 青岛科技大学 | Preparation method of zinc oxide with core-shell structure and zinc oxide obtained by preparation method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1288861A (en) * | 2000-08-25 | 2001-03-28 | 山东省海洋化工科学研究院 | Method for preparing metal oxide nano material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1288861A (en) * | 2000-08-25 | 2001-03-28 | 山东省海洋化工科学研究院 | Method for preparing metal oxide nano material |
Non-Patent Citations (2)
| Title |
|---|
| CaO–ZnO Catalyst for Selective Conversion of Methane to C2 Hydrocarbons Using Carbon Dioxide as the Oxidant;Ye Wang等;《Journal of Catalysis》;20001231;第252–255页 * |
| Ye Wang等.CaO–ZnO Catalyst for Selective Conversion of Methane to C2 Hydrocarbons Using Carbon Dioxide as the Oxidant.《Journal of Catalysis》.2000,第252–255页. |
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