CN102390862A - Liquid-phase precipitation preparation method of zinc oxide porous hollow balls - Google Patents
Liquid-phase precipitation preparation method of zinc oxide porous hollow balls Download PDFInfo
- Publication number
- CN102390862A CN102390862A CN2011102322557A CN201110232255A CN102390862A CN 102390862 A CN102390862 A CN 102390862A CN 2011102322557 A CN2011102322557 A CN 2011102322557A CN 201110232255 A CN201110232255 A CN 201110232255A CN 102390862 A CN102390862 A CN 102390862A
- Authority
- CN
- China
- Prior art keywords
- porous hollow
- zinc oxide
- liquid
- hollow balls
- oxide porous
- 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.)
- Pending
Links
Images
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a liquid-phase precipitation preparation method of zinc oxide porous hollow balls. The method is characterized in that hexamethylentetramine and zinc nitrate are used as raw materials, sodium citrate is used as a surfactant, and precipitation reaction is carried out in water. The method comprises the following steps of: 1) dissolving hexamethylentetramine in deionized water, and adding zinc nitrate and sodium citrate to obtain a reaction solution; and 2) placing the reaction solution in a 80-95 DEG C water bath tank, reacting for 3-7 hours, carrying out suction filtering to obtain white precipitate, sufficiently washing the precipitate, filtering, and drying the precipitate to obtain powdery zinc oxide porous hollow balls. The method has the advantages and positive effects that: 1) compared with other methods, the liquid-phase precipitation preparation method of ZnO porous hollow balls has simple process and low cost; and 2) uniformly distributed ZnO porous hollow balls obtained by the method have large specific surface area and can sufficiently contact gas by virtue of the porous structure, thereby particularly facilitating the manufacture of gas-sensitive devices based on ZnO nanomaterial.
Description
Technical field
The invention belongs to the preparation that belongs to gas sensitive, particularly a kind of liquid-phase precipitation method prepares the method for ZnO porous hollow sphere.
Background technology
Zinc oxide is a kind of important wide bandgap compound semiconductors, has important use in fields such as chemical sensor, piezoelectricity, photochemical catalysis, opto-electronic conversion, blue green LED and laser apparatus and is worth.In chemical sensor, piezoelectricity, photochemical catalysis, opto-electronic conversion application process, increase the zinc oxide specific surface area is to promote its performance effective ways always.The method for preparing zinc oxide commonly used at present; Like template, sol-gel method, microemulsion method etc.; The common only outside surface of material capable of using; Do not give full play to the performance of material as yet, the zinc oxide porous hollow sphere that this patent proposed passes the internal surface and the outside surface that can make full use of material, might realize improving the above-mentioned application performance of material.
Summary of the invention
The objective of the invention is according to above-mentioned technical Analysis, the method that provides a kind of liquid-phase precipitation method to prepare the zinc oxide porous hollow sphere, this preparing method's technology is simple, cost is low, and can obtain equally distributed ZnO nanoporous hollow ball, and specific surface area is bigger; This material is used to prepare the heater-type gas sensor, can fully contact with monitoring gas.
Technical scheme of the present invention:
A kind of liquid-phase precipitation method prepares the method for zinc oxide porous hollow sphere
,With hexamethylenetetramine and zinc nitrate is raw material, is tensio-active agent with the Trisodium Citrate, in water, carries out precipitin reaction, and step is following:
1) hexamethylenetetramine is dissolved in the deionized water, ultrasonic it is dissolved fully, add zinc nitrate and fully after the dissolving, add Trisodium Citrate again, process reaction solution;
2) reaction solution is placed suction filtration behind 80～95 ℃ of water baths reaction 3-7h; Obtain white depositions; Throw out is used deionized water, absolute ethyl alcohol thorough washing respectively, after the filtration throw out is dried under 50～80 ℃ of temperature, can make the powdered zinc oxide porous hollow sphere.
The amount ratio of said hexamethylenetetramine, zinc nitrate, Trisodium Citrate and deionized water is that hexamethylenetetramine is that 0.1-0.4g, zinc nitrate are that 0.5-0.8 g, Trisodium Citrate are 0.1-0.2g in the 100 ml deionized waters.
Reaction principle of the present invention: when no Trisodium Citrate exists; Zinc oxide is easy to form club shaped structure; But owing to there is Trisodium Citrate; Regular chain-like structure makes it be easy to be adsorbed on its process of growth of ZnO surface of seed change, causes the formation of sheet structure, and the continuous gathering of sheet structure has finally formed the surface and has been the ZnO porous hollow sphere of porous laminated structure.The surface of ZnO porous hollow sphere is to combine porous laminated structure by many particles, and the space is arranged again between the particle, and some ball surface does not have complete closed; Part is opened wide, and the diameter of ball is about 2 μ m, and gas molecule can get into; Inside and outsidely all can contact simultaneously with gas; Thereby the adsorb oxygen amount that has improved nano zine oxide reaches the contact area with gas, and it is had good air-sensitive performance as gas sensitive, can be used as gas sensitive and is applied to gas sensing unit.
Advantage of the present invention and positively effect:
1) liquid-phase precipitation method prepares the preparation method and the data by MoM and MEI of ZnO porous hollow sphere, and technology is simple, cost is low; 2) this method can obtain equally distributed ZnO porous hollow sphere, and specific surface area is bigger, and vesicular structure fully contacts its gas, and this is particularly conducive to the manufacturing based on the gas sensitive device of ZnO nano material.
[description of drawings]
Fig. 1 is a ZnO porous hollow sphere ball wall SEM photo, and illustration is a porous hollow sphere SEM photo.
Fig. 2 is the XRD figure of ZnO porous hollow sphere.
Fig. 3 is the nitrogen adsorption/desorption isothermal curve of ZnO porous hollow sphere.
Fig. 4 is the sensitivity curve of ZnO porous hollow sphere to different concentration ethanol.
[embodiment]
Embodiment:
A kind of liquid-phase precipitation method prepares the method for zinc oxide porous hollow sphere
,With hexamethylenetetramine and zinc nitrate is raw material, is tensio-active agent with the Trisodium Citrate, in water, carries out precipitin reaction, and step is following:
1) the 0.7g hexamethylenetetramine is dissolved in the 200ml deionized water, ultrasonic it is dissolved fully, add the 1.49g zinc nitrate again, after the dissolving, take by weighing the 0.24g Trisodium Citrate again and add above-mentioned solution fully, it is dissolved fully.
2) this mixing solutions is placed 95 ℃ of water baths, reaction back suction filtration gets white precipitate, for observing its process of growth, has set 3 reaction times, is respectively 3h, 5h and 7h.After reaction finishes respectively with throw out with deionized water, absolute ethyl alcohol thorough washing, after the filtration throw out is placed 60 ℃ of baking ovens dryings, make Powdered ZnO porous hollow sphere.Whether can influence product structure for observing annealing process, the product that makes was calcined 2 hours in 400 ℃ of retort furnaces.
Fig. 1, Fig. 2 and Fig. 3 are respectively to be ZnO porous hollow sphere SEM, XRD, the nitrogen adsorption/desorption isothermal curve of 5h in the reaction times.Can know that by Fig. 1 the surface of ball is to combine porous laminated structure by many particles, thickness is about about 10nm, and the space is arranged between the particle.Can know the wurtzite structure that is of ZnO porous hollow sphere through the preparation of this method by Fig. 2, crystallization degree is very high.The specific surface area that is obtained product by nitrogen adsorption/desorption isothermal curve of Fig. 3 is 41.84 m
2/ g.Fig. 4 ZnO differential responses time porous hollow sphere is to alcoholic acid sensitivity curve figure, and 5h is the suitable reactions time, and sensitivity is 51.4 to product to the 500ppm alcoholic acid at this moment.
Claims (2)
1. a liquid-phase precipitation method prepares the method for zinc oxide porous hollow sphere
,It is characterized in that: with hexamethylenetetramine and zinc nitrate is raw material, is tensio-active agent with the Trisodium Citrate, in water, carries out precipitin reaction, and step is following:
1) hexamethylenetetramine is dissolved in the deionized water, ultrasonic it is dissolved fully, add zinc nitrate and fully after the dissolving, add Trisodium Citrate again, process reaction solution;
2) reaction solution is placed suction filtration behind 80～95 ℃ of water baths reaction 3-7h; Obtain white depositions; Throw out is used deionized water, absolute ethyl alcohol thorough washing respectively, after the filtration throw out is dried under 50～80 ℃ of temperature, can make the powdered zinc oxide porous hollow sphere.
2. the method for preparing the zinc oxide porous hollow sphere according to the said liquid-phase precipitation method of claim 1
,It is characterized in that: the amount ratio of said hexamethylenetetramine, zinc nitrate, Trisodium Citrate and deionized water is that hexamethylenetetramine is that 0.1-0.4g, zinc nitrate are that 0.5-0.8 g, Trisodium Citrate are 0.1-0.2g in the 100 ml deionized waters.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102322557A CN102390862A (en) | 2011-08-15 | 2011-08-15 | Liquid-phase precipitation preparation method of zinc oxide porous hollow balls |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102322557A CN102390862A (en) | 2011-08-15 | 2011-08-15 | Liquid-phase precipitation preparation method of zinc oxide porous hollow balls |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102390862A true CN102390862A (en) | 2012-03-28 |
Family
ID=45858273
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011102322557A Pending CN102390862A (en) | 2011-08-15 | 2011-08-15 | Liquid-phase precipitation preparation method of zinc oxide porous hollow balls |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102390862A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102897825A (en) * | 2012-09-25 | 2013-01-30 | 江苏大学 | Method for preparing nano-hollow spherical shell zinc oxide by hydrothermal-calcinating method |
| CN103943838A (en) * | 2014-04-21 | 2014-07-23 | 西安交通大学 | Preparation method of metal oxide nanosheet and carbon nanotube composite energy-storage material |
| CN104128159A (en) * | 2014-08-13 | 2014-11-05 | 陕西科技大学 | Wastewater treatment material with photocatalysis and heavy metal adsorption functions and capable of being recycled and preparation method thereof |
| CN104164176A (en) * | 2014-08-04 | 2014-11-26 | 陕西科技大学 | Method for enhancing water resistance of water-based polyurethane for synthetic leather by using zinc oxide |
| CN105600815A (en) * | 2014-11-12 | 2016-05-25 | 天津科技大学 | Doped nanometer zinc oxide light conversion agent preparation method |
| CN107572578A (en) * | 2017-09-07 | 2018-01-12 | 东南大学 | A kind of method that no template prepares zinc oxide spherical shell |
| CN109174092A (en) * | 2018-09-21 | 2019-01-11 | 东华大学 | A kind of zinc oxide/platinum composite material microballoon and its preparation method and application |
| CN110002511A (en) * | 2019-04-18 | 2019-07-12 | 郑州轻工业学院 | A kind of Co of hollow structure3O4Nano material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101311119B (en) * | 2007-05-25 | 2010-09-08 | 中国科学院合肥物质科学研究院 | Reticular nano hole zinc oxide micron hollow ball and preparation method thereof |
| CN101948130A (en) * | 2010-10-11 | 2011-01-19 | 厦门大学 | Zinc oxide hollow microspheres and preparation method thereof |
-
2011
- 2011-08-15 CN CN2011102322557A patent/CN102390862A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101311119B (en) * | 2007-05-25 | 2010-09-08 | 中国科学院合肥物质科学研究院 | Reticular nano hole zinc oxide micron hollow ball and preparation method thereof |
| CN101948130A (en) * | 2010-10-11 | 2011-01-19 | 厦门大学 | Zinc oxide hollow microspheres and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| MING WANG ET AL.: "Template-free fabrication of porous zinc oxide hollow spheres and their enhanced photocatalytic performance", 《J POROUS MATER》 * |
| 蔡锋石 等: "分级多孔结构ZnO微球的制备及其光电性能", 《无机化学学报》 * |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102897825B (en) * | 2012-09-25 | 2014-05-28 | 江苏大学 | Method for preparing nano-hollow spherical shell zinc oxide by hydrothermal-calcinating method |
| CN102897825A (en) * | 2012-09-25 | 2013-01-30 | 江苏大学 | Method for preparing nano-hollow spherical shell zinc oxide by hydrothermal-calcinating method |
| CN103943838B (en) * | 2014-04-21 | 2016-07-20 | 西安交通大学 | The preparation method of metal oxide nano-sheet and CNT composite energy-storage material |
| CN103943838A (en) * | 2014-04-21 | 2014-07-23 | 西安交通大学 | Preparation method of metal oxide nanosheet and carbon nanotube composite energy-storage material |
| CN104164176A (en) * | 2014-08-04 | 2014-11-26 | 陕西科技大学 | Method for enhancing water resistance of water-based polyurethane for synthetic leather by using zinc oxide |
| CN104128159A (en) * | 2014-08-13 | 2014-11-05 | 陕西科技大学 | Wastewater treatment material with photocatalysis and heavy metal adsorption functions and capable of being recycled and preparation method thereof |
| CN104128159B (en) * | 2014-08-13 | 2016-04-20 | 陕西科技大学 | There is wastewater treatment material that photocatalysis and heavy metal adsorption function can be recycled and preparation method thereof |
| CN105600815A (en) * | 2014-11-12 | 2016-05-25 | 天津科技大学 | Doped nanometer zinc oxide light conversion agent preparation method |
| CN105600815B (en) * | 2014-11-12 | 2018-04-20 | 天津科技大学 | A kind of preparation method of doped nano zinc oxide light conversion agent |
| CN107572578A (en) * | 2017-09-07 | 2018-01-12 | 东南大学 | A kind of method that no template prepares zinc oxide spherical shell |
| CN109174092A (en) * | 2018-09-21 | 2019-01-11 | 东华大学 | A kind of zinc oxide/platinum composite material microballoon and its preparation method and application |
| CN109174092B (en) * | 2018-09-21 | 2021-07-20 | 东华大学 | Zinc oxide/platinum composite material microsphere and preparation method and application thereof |
| CN110002511A (en) * | 2019-04-18 | 2019-07-12 | 郑州轻工业学院 | A kind of Co of hollow structure3O4Nano material and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102390862A (en) | Liquid-phase precipitation preparation method of zinc oxide porous hollow balls | |
| CN109709192B (en) | Gas-sensitive nanomaterial based on tungsten oxide/tin oxide core-shell nanosheet structure, preparation process and application thereof | |
| Zhang et al. | MIL-125 (Ti)-derived COOH functionalized TiO2 grafted molecularly imprinted polymers for photoelectrochemical sensing of ofloxacin | |
| CN107364897A (en) | A kind of preparation method of ferrous acid zinc nano material | |
| CN108190970A (en) | A kind of preparation method and applications of Co-doped ZnO gas sensitive | |
| CN100480428C (en) | Ultra-hydrophobic high sticking composite metal oxide thin film and preparing method thereof | |
| CN105271371B (en) | A kind of flower-shaped indium oxide micron bar material and its preparation method and application | |
| CN103950969A (en) | Preparation method of multistage porous metal oxide nano-material | |
| CN102041553A (en) | Preparation method and application of crystalline-state beta-MnOOH nanowire | |
| CN107449805B (en) | Acetone-sensitive zinc cobaltate nano multi-shell yolk-shell membrane | |
| CN110065972B (en) | Preparation of hamburger-shaped Co from ZIF-673O4Method for producing gas-sensitive material and use thereof | |
| CN110498440A (en) | A kind of zinc oxide air-sensitive membrane material, preparation method and applications | |
| CN102320648A (en) | Preparation method and application of lanthanum ion-doped zinc oxide porous hollow sphere | |
| Arif et al. | Ag functionalized In2O3 derived from MIL-68 (in) as an efficient electrochemical glucose sensor | |
| CN113912104A (en) | Two-dimensional porous CeOx/SnO2Nanosheet and preparation method and application thereof | |
| CN109499582B (en) | Composite oxide mimic enzyme material and preparation method and application thereof | |
| CN109732099B (en) | Preparation method of antioxidant micron copper | |
| CN117069165A (en) | Preparation method of Pd modified two-dimensional porous NiO/ZnO gas-sensitive material and method for preparing CO gas sensor by using Pd modified two-dimensional porous NiO/ZnO gas-sensitive material | |
| CN103074627A (en) | Method for preparing composite semiconductor sensitive film based on replacement reaction-thermal oxidation method | |
| CN116593538A (en) | GaN/rGO ammonia sensor and preparation method thereof | |
| CN114507353B (en) | Preparation method and application of organic hybrid perovskite/metal organic framework material | |
| CN114988457A (en) | Based on alpha-Fe 2 O 3 Nanowire heteroepitaxy ZnO @ ZIF-8 microporous nanomaterial, and preparation process and application thereof | |
| CN112964758B (en) | Manganese dioxide nanosheet/titanium dioxide nanowire array composite resistance type sensor and preparation method and application thereof | |
| CN113624808A (en) | Three-dimensional radial cobaltosic oxide nanowire cluster sensitive to acetone gas | |
| CN101311359A (en) | Preparation method of cuboid indium oxide single crystal |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120328 |