CN103214026A - Preparation method of CaO/ZnO core-shell structure nanometer material - Google Patents
Preparation method of CaO/ZnO core-shell structure nanometer material Download PDFInfo
- Publication number
- CN103214026A CN103214026A CN2013101758248A CN201310175824A CN103214026A CN 103214026 A CN103214026 A CN 103214026A CN 2013101758248 A CN2013101758248 A CN 2013101758248A CN 201310175824 A CN201310175824 A CN 201310175824A CN 103214026 A CN103214026 A CN 103214026A
- Authority
- CN
- China
- Prior art keywords
- cao
- zno
- shell structured
- nuclear shell
- structured nano
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Luminescent Compositions (AREA)
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 the 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
The nuclear shell structured nano-material is used widely multi-field because of nuclear core composition and 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 for preparing the nuclear shell structured nano-material has a lot, and template has efficient, easy characteristics and often is used to prepare spherical nuclear shell structured nano-material.Mould material commonly used has a lot, comprises silicon ball, polystyrene emulsion and soft template etc. as hard template.Nanometer CaCO
3Have stronger perviousness, be used widely at aspects such as pigment, opticglass, pottery and electrical condenser preparations.CaCO
3Microballoon can be particularly suitable for preparing the nucleocapsid structure microballoon as template, with CaCO by being decomposed to form CaO
3Nanometer ball does not appear in the newspapers as yet as the research that template prepares CaO/ZnO nuclear shell structured nano-material.
At present, ZnO is used widely in a lot of fields as the 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 preparation ZnO.Synthetic environment such as form conditioning agent and reaction medium can influence the microstructure of ZnO, bibliographical information, and synthetic rule nano-ZnO can present different structures, as bar-shaped, nano wire, star, quadrangle, flower shape, sphere and height symmetrical structure etc.But, less about the research report of preparation CaO/ZnO nuclear shell structured nano-material, to compare 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, with CaCO
3Nanometer ball is distributed to H
2In the mixed solution of O and DMF; Again with Zn (AcO)
2Join in the mixed solution continuously stirring; The room temperature ageing; Centrifugal collecting precipitation: vacuum-drying; By high-temperature calcination, form the CaO/ZnO nuclear shell structured nano-material of different shapes such as sphere or class sphere.
The present invention prepares CaO/ZnO nuclear shell structured nano-material by the precipitator method in the easy liquid, and this material has nuclear 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 the liquid, after high-temperature calcination, promptly obtains CaO/ZnO nuclear shell structured nano-material.
CaO/ZnO nuclear shell structured nano-preparation methods:
(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) with Zn (AcO)
2Join in the 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) normal temperature vacuum-drying 12～72h;
(6) 450～830 ℃ of calcining 1～3h, the nano material of formation CaO/ZnO composite structure.
Nanometer CaCO
3Available from Shanghai reagent company.Zinc acetate (Zn (AcO)
2) and N, N dimethyl formamide (DMF) is an analytical pure, does not need purifying during application, all the water that uses in the experimentation is deionized water.Under normal temperature and pressure conditions, forming process, form and the structure of product are characterized by XRD, SEM and TEM.
Method provided by the invention is compared with existing preparation method and had the following advantages and the high-lighting effect: the nuclear shell structured nano-material product form and the structure of this method preparation can be regulated and control; Productive rate is higher; Technology is simple, easy to operate, is beneficial to industrialization.
Description of drawings
The XRD spectra of the CaO/ZnO nuclear shell structured nano-material of Fig. 1: embodiment 1 preparation illustrates to include CaO and ZnO in the prepared material;
Fig. 2: the CaO/ZnO nuclear shell structured nano-material TEM photo of different Zn/Ca mol ratios (Fig. 2 a5:1, Fig. 2 b7:1) preparation;
Fig. 3: the CaO/ZnO nuclear shell structured nano-material TEM photo of differential responses temperature (Fig. 3 a450 ℃, Fig. 3 b830 ℃) preparation;
Fig. 4: different H
2The CaO/ZnO nuclear shell structured nano-material TEM photo of the volume ratio of O/DMF (Fig. 4 a8:2, Fig. 4 b7:3) preparation.
Embodiment
CaO/ZnO nuclear shell structured nano-material with nuclear core composition CaO and shell composition ZnO is to prepare by the precipitator method in the easy liquid.With CaCO
3Nanometer ball is distributed in the mixed solution of water and DMF, zinc acetate is joined in the mixed solution again, continues to stir.Through high-temperature calcination, obtain CaO/ZnO nuclear shell structured nano-material.
Further specify CaO/ZnO nuclear shell structured nano-preparation methods of the present invention and characteristics thereof below by several exemplary embodiments.
1, the CaO/ZnO nuclear shell structured nano-material of different Zn/Ca mol ratio preparations
Embodiment 1:
CaCO
3Nanometer ball (particle diameter 60-80nm) is distributed to H
2In the mixed solution of O and DMF, then, with the Zn (AcO) of difference amount
2(calculating with the 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 the Zn/Ca mol ratio was 5:1, the form of prepared CaO/ZnO nuclear shell structured nano-material was stub shape or class sphere, the slight gathering.The 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, the microballoon good dispersity, and the thickness of ZnO shell is about 50nm.
2, the CaO/ZnO nuclear shell structured nano-material of different calcining temperature preparations
Embodiment 2:
CaCO
3Nanometer ball is distributed to H
2In the mixed solution of O and DMF, with 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 ℃, 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 ℃, 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
2The CaO/ZnO nuclear shell structured nano-material of the volume ratio preparation of O/DMF
Embodiment 3:
CaCO
3Nanometer ball is distributed to H
2O and DMF(different volumes than) mixed solution in, then, with 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
2The O/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.
Above in conjunction with specific embodiments, the present invention has been done further elaboration, rather than 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 the easy liquid, is with CaCO
3Nano material is distributed in the mixed solution of water and DMF, zinc acetate joins in the mixed solution, continuously stirring, through high-temperature calcination, obtain CaO/ZnO nuclear shell structured nano-material, this material has nuclear core composition CaO and shell composition ZnO, as for other mould materials beyond the Application Example, solvent material, nuclear core material, shell material, digestion time, calcining temperature, time etc. all in design scope of the present invention.
Claims (7)
1. CaO/ZnO nuclear shell structured nano-preparation methods, its step is as follows:
(1) with 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;
(2) with Zn (AcO)
2Join in the above-mentioned mixed solution, the mol ratio that makes Zn/Ca is 5:1～7:1, continuously stirring;
(3) room temperature ageing;
(4) centrifugal collecting precipitation;
(5) normal temperature vacuum-drying;
(6) obtain CaO/ZnO nuclear shell structured nano-material after the calcining.
2. a kind of CaO/ZnO nuclear shell structured nano-preparation methods as claimed in claim 1 is characterized in that: in the middle mixed solution of step (1), and CaCO
3Concentration be 0.08～0.10mol/L.
3. a kind of CaO/ZnO nuclear shell structured nano-preparation methods as claimed in claim 1 is characterized in that: the time of stirring in the step (1) is 10～18h.
4. a kind of CaO/ZnO nuclear shell structured nano-preparation methods as claimed in claim 1 is characterized in that: the aged time of room temperature is 12～36h in the step (3).
5. a kind of CaO/ZnO nuclear shell structured nano-preparation methods as claimed in claim 1 is characterized in that: centrifugal speed is 3000～8000rpm in the step (4).
6. a kind of CaO/ZnO nuclear shell structured nano-preparation methods as claimed in claim 1 is characterized in that: the vacuum drying time is 12～72h in the step (5).
7. a kind of CaO/ZnO nuclear shell structured nano-preparation methods as claimed in claim 1 is characterized in that: the incinerating temperature is 450～830 ℃ in the step (6), and the incinerating time is 1～3h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310175824.8A CN103214026B (en) | 2013-05-13 | 2013-05-13 | Preparation method of CaO/ZnO core-shell structure nanometer material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310175824.8A CN103214026B (en) | 2013-05-13 | 2013-05-13 | Preparation method of CaO/ZnO core-shell structure nanometer material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103214026A true CN103214026A (en) | 2013-07-24 |
| CN103214026B CN103214026B (en) | 2014-07-16 |
Family
ID=48812253
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310175824.8A Expired - Fee Related CN103214026B (en) | 2013-05-13 | 2013-05-13 | Preparation method of CaO/ZnO core-shell structure nanometer material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103214026B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106924052A (en) * | 2017-03-24 | 2017-07-07 | 吉林大学 | A kind of CaO nano particle antibacterial materials with ZnO coatings 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 |
| CN111606351A (en) * | 2020-05-21 | 2020-09-01 | 江南大学 | Zinc oxide coated calcium carbonate nano material and preparation method thereof |
| CN114436320A (en) * | 2022-01-25 | 2022-05-06 | 青岛科技大学 | Preparation method of core-shell structure zinc oxide 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 |
-
2013
- 2013-05-13 CN CN201310175824.8A patent/CN103214026B/en not_active Expired - Fee Related
Patent 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 |
Non-Patent Citations (1)
| Title |
|---|
| YE WANG等: "CaO–ZnO Catalyst for Selective Conversion of Methane to C2 Hydrocarbons Using Carbon Dioxide as the Oxidant", 《JOURNAL OF CATALYSIS》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106924052A (en) * | 2017-03-24 | 2017-07-07 | 吉林大学 | A kind of CaO nano particle antibacterial materials with ZnO coatings 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 |
| CN111606351A (en) * | 2020-05-21 | 2020-09-01 | 江南大学 | Zinc oxide coated calcium carbonate nano material and preparation method thereof |
| CN111606351B (en) * | 2020-05-21 | 2021-08-24 | 江南大学 | Zinc oxide coated calcium carbonate nano material and preparation method thereof |
| CN114436320A (en) * | 2022-01-25 | 2022-05-06 | 青岛科技大学 | Preparation method of core-shell structure zinc oxide and zinc oxide obtained by preparation method |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103214026B (en) | 2014-07-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| TWI458685B (en) | Titanium dioxide nanopowder and manufacturing method thereof | |
| CN109502632B (en) | Multistage SnO2Preparation method and application of nanotube-shaped gas-sensitive material | |
| CN105060351B (en) | Flower-like cobaltosic oxide material composed of nanoparticles and preparation method thereof | |
| CN103214026B (en) | Preparation method of CaO/ZnO core-shell structure nanometer material | |
| CN103359773B (en) | A kind of preparation method of zinc oxide nano rod | |
| CN104003448A (en) | [Alpha]-phase ferric oxide porous core-shell microspheres and controllable synthetic preparation method thereof | |
| An et al. | Facile template-free synthesis and characterization of elliptic α-Fe2O3 superstructures | |
| CN103011306A (en) | Method for preparing nano-scale cubic cobaltosic oxide | |
| WO2021104087A1 (en) | Metal oxide nanoparticles, and preparation method therefor and application thereof | |
| CN105129849A (en) | Flowerlike nano-sized titanium dioxide material and template-free preparation method thereof | |
| CN103435097B (en) | Preparation method and application of nano zirconia | |
| CN108238605A (en) | A kind of three-dimensional flower-shaped alkali formula silicic acid nickel microballoon and preparation method thereof | |
| CN103643350B (en) | A kind of Co 3o 4/ In 2o 3heterogeneous structural nano pipe and preparation method thereof and application | |
| CN111233048A (en) | Double-shell MnCo2O4Hollow nanosphere material and synthesis method thereof | |
| CN105585043A (en) | Preparation method of flowerlike cerium oxide nano-material | |
| CN105800604A (en) | Preparation method of graphene-loaded cobalt ferrite quantum dot | |
| CN101941677B (en) | Method for preparing manganese oxide surface modified zinc oxide nano rod | |
| CN108262041A (en) | A kind of one pot of method for preparing high activity gold/zinc oxide compound nano cluster of room temperature | |
| CN104001489A (en) | High-photocatalytic-activity flower-shaped porous titanium dioxide nano material and preparation method thereof | |
| CN103833080A (en) | Preparation method for cadmium molybdate porous spheres | |
| CN103331452B (en) | Copper and carbon composite hollow sphere particle material and preparation method thereof | |
| Zhang et al. | Facile synthesis of well-defined CeO2 hollow spheres with a tunable pore structure | |
| CN105712401B (en) | Calcium vanadate sphere material and its preparation method and application | |
| CN104140123A (en) | Three-dimensional flower-shaped titanic acid material formed by assembling lamelleted nanosheets and synthesizing method of three-dimensional flower-shaped titanic acid material | |
| CN105036188B (en) | A kind of titanium dioxide nano thread and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140716 Termination date: 20180513 |