CN103241959A - Preparation method of Na-doped ZnO nanorod array - Google Patents
Preparation method of Na-doped ZnO nanorod array Download PDFInfo
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- CN103241959A CN103241959A CN2013101590957A CN201310159095A CN103241959A CN 103241959 A CN103241959 A CN 103241959A CN 2013101590957 A CN2013101590957 A CN 2013101590957A CN 201310159095 A CN201310159095 A CN 201310159095A CN 103241959 A CN103241959 A CN 103241959A
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Abstract
The invention relates to the technical field of optical materials and in particular relates to a preparation method of a Na-doped ZnO nanorod array. The preparation method comprises the following steps of: preparing a ZnO seed precursor by utilizing a sol-gel method; coating the ZnO precursor on a substrate to form a film; and placing the film to a mixed solution of sodium chloride, zinc acetate dihydrate and hexamine to grow a uniform nanorod array in a hydrothermal reaction container. The preparation method of the Na-doped ZnO nanorod array is simple and easy to implement, simple in equipment, high in yield, low in cost, controllable in diameter and length of the obtained ZnO nanorod array and good in optical performances.
Description
Technical field
The present invention relates to the optical material technical field, more specifically, relate to a kind of preparation method of Na doping zinc oxide nanometer rod array.
Background technology
ZnO is a kind of important direct semiconductor material with wide forbidden band, and its energy gap is 3.37 eV under the room temperature, has bigger exciton bind energy (60 meV).Simultaneously it also is a kind of multi-functional oxidation thing material, all has excellent performance in photoelectricity, piezoelectricity, thermoelectricity, every field such as ferroelectric and ferromagnetic, has been widely used on surface acoustic wave device, solar cell, air-sensitive, the pressure-sensitive and photoelectric device.Because raw material resources is abundant, low price, to the environment toxicological harmless, so become after GdN another research focus in the world in recent years.Since people such as calendar year 2001 Huang observe Ultra-Violet Laser emission back (M. Huang, S. Mao, H. Feick under optical pumping excites in the synthetic ZnO nanometer stick array of sapphire substrates and the environment in room temperature, H. Yan, Y. Wu, H. Kind, E. Weber, R. Russo, P. Yang, Science, 2001,292:1897-l899), ZnO nanometer stick array Luminescence Study of Modified Porous becomes the focus of common concern in the world.The preparation method of ZnO nanometer stick array mainly contains chemical gas-phase method, electrochemical deposition method and hydrothermal method etc.Wherein chemical gas-phase method and electrochemical deposition method energy consumption height, conversion unit costliness, severe reaction conditions, complicated operation.Hydrothermal method is simple because of its required equipment, and temperature of reaction is low, and is easy to operate, is fit to scale operation and enjoys people to adopt.
Summary of the invention
The present invention is for overcoming the described at least a defective of above-mentioned prior art, a kind of hydrothermal method of utilizing is provided, cost is low, efficient is high, can be used for big area and produce the preparation method of high quality Na doping zinc oxide nanometer rod array, utilize the doping of sodium-chlor to regulate and control structure and the pattern of ZnO nanometer stick array, obtain the ZnO nanometer stick array with favorable optical performance.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of Na doping zinc oxide nanometer rod array wherein, may further comprise the steps:
S1. substrate is cleaned: substrate is successively with acetone, alcohol, deionized water ultrasonic cleaning and oven dry, standby;
S2. ZnO Seed Layer precursor solution preparation: a certain amount of zinc acetate and thanomin are joined in the ethylene glycol monomethyl ether successively, after fully stirring, make ZnO Seed Layer precursor solution after the sealing homogenizing;
S3. ZnO Seed Layer preparation: the substrate after will cleaning is transferred on the equal glue machine, drips ZnO Seed Layer precursor solution, is coated with after treating evenly to disperse, and anneal is carried out in the substrate that will be coated with ZnO Seed Layer precursor solution after the drying;
S4. the configuration of growth solution: hexamethylenetetramine, Zinc diacetate dihydrate and sodium-chlor are added in the deionized water, stir, obtain growth media;
S5. the preparation of ZnO nanometer stick array: the substrate that will contain the ZnO Seed Layer is immersed in the growth media, at 90 ℃ of growth 2～48 h down, and naturally cooling then, the rear film of will grow is rinsed the back drying well with deionized water, makes the ZnO nanometer stick array.
Further, described substrate is silicon chip, sapphire, quartz or slide glass.
Further, among the described step S2, the volumetric molar concentration of zinc acetate and thanomin is 75mM.
Further, among the described step S2, the time of sealing homogenizing is 24h.
Further, among the described step S3, the process that is coated with is for starting sol evenning machine, and 500 rpm are coated with 20 s, are coated with 60 s with 5000 rpm again, 120 ℃ of following dry 15 min.The process repetitive operation that is coated with 4 times.
Further, among the described step S3, anneal is in retort furnace, carries out anneal 2 h under 360 ℃.
Further, among the described step S4, the volumetric molar concentration of hexamethylenetetramine and Zinc diacetate dihydrate is 12.5mM, and deionized water is 10ml.
Further, among the described step S4, sodium-chlor is 0.0409 g or 0.0818 g or 0.1227 g or 0.1636 g.
Along with the increase of sodium-chlor doping content, move toward the Small angle direction gradually the diffraction peak position, and this is because the ratio of ionic radii Zn of Na big, and after Na replaced the position of Zn, spacing increased.
The nanometer rod of Hydrothermal Growth preparation is evenly gathered on silicon chip substrate, grows to arrange along the direction perpendicular to silicon chip substrate to form neat nanometer rod, and direction of growth unanimity, the size homogeneous, and also the top of each nanometer rod is smooth with the surface.Pure ZnO nanometer stick array diameter is 30 nm, and length is 750 nm.Along with the increase of sodium-chlor doping content, the nanometer one-dimensional array is more and more intensive, be close to be tiled in the silicon chip substrate surface fully, and because the shortening of length, the directivity of one-dimensional array is more excellent.The doping of sodium-chlor is 0.0409g, and when 0.0818g and 0.1227 g and 0.1636g, the diameter of nanometer rod is respectively 50 nm, 60 nm, and 70 nm and 70 nm, length is respectively 150 nm, 112 nm, 98 nm and 71 nm.As seen along with the increase of sodium-chlor doping content, the diameter of nanometer rod increases gradually, and length then reduces gradually.
Compared with prior art, beneficial effect is: the present invention is cheap, operational safety, and environmental friendliness, good reproducibility, structure and the pattern of Na doping zinc oxide nanometer rod array are controlled, and the luminescent properties excellence.Prepared nanometic zinc oxide rod array can be used for fields such as gas sensitive, sensor, photo-detector.
Description of drawings
Fig. 1 is the XRD figure of the asynchronous sample of doping of sodium-chlor of the present invention.
Fig. 2 is the SEM figure of the asynchronous sample of doping of sodium-chlor of the present invention.
Fig. 3 is the PL figure of the asynchronous sample of doping of sodium-chlor of the present invention.
Embodiment
Accompanying drawing only is used for exemplary illustration, can not be interpreted as the restriction to this patent; For better explanation present embodiment, some parts of accompanying drawing have omission, amplify or dwindle, and do not represent the size of actual product; To those skilled in the art, in the accompanying drawing some known features and explanation thereof may to omit be understandable.The present invention adopts single or multiple micro display chip arrays, based on spatial reuse and time-division multiplex technology, realizes with great visual angle interactive even full visual angle true three-dimension image display system.
In the present embodiment, a kind of preparation method of Na doping zinc oxide nanometer rod array wherein, may further comprise the steps:
S1. substrate is cleaned: substrate is successively with acetone, alcohol, deionized water ultrasonic cleaning and oven dry, standby;
S2. ZnO Seed Layer precursor solution preparation: zinc acetate and the thanomin (volumetric molar concentration is 75 mM) of equimolar amount are joined in the ethylene glycol monomethyl ether successively, and after fully stirring, sealing homogenizing 24 h make ZnO Seed Layer precursor solution;
S3. ZnO Seed Layer preparation: the substrate after will cleaning is transferred on the equal glue machine, drips ZnO Seed Layer precursor solution, after treating evenly to disperse, starts sol evenning machine, and 500 rpm are coated with 20 s, are coated with 60 s with 5000 rpm again, dry 15 min under 120 ℃.Repeat aforesaid operations 4 times to increase film thickness.The substrate that will be coated with ZnO Seed Layer precursor solution is at last transferred in the retort furnace, carries out anneal 2 h under 360 ℃;
S4. the configuration of growth solution: the sodium-chlor of equimolar hexamethylenetetramine and Zinc diacetate dihydrate (volumetric molar concentration is 12.5 mM) and 0.0409 g or 0.0818 g or 0.1227 g or 0.1636 g is added in the 10 ml deionized waters, stir, obtain growth media;
S5. the preparation of ZnO nanometer stick array: the substrate that will contain the ZnO Seed Layer is immersed in the growth media, and at 90 ℃ of 2 h that grow down, the rear film of will growing is rinsed the back drying well with deionized water, makes the ZnO nanometer stick array.
As shown in Figure 1, the doping of sodium-chlor is (a) 0 g, (b) 0.0409 g, (c) 0.0818 g, (d) 0.1227 g and (e) XRD figure of sample during 0.1636 g.
As shown in Figure 2, the doping of sodium-chlor is (a, b) 0 g, (c) 0.0409 g, (d) 0.0818 g, (e) 0.1227 g and (f) SEM of sample figure during 0.1636 g.Illustration is the sectional view of respective sample.Scale: 500 nm.
As shown in Figure 3, the doping of sodium-chlor is (a) 0 g, (b) 0.0409 g, (c) 0.0818 g, (d) 0.1227 g and (e) PL of sample figure during 0.1636 g.
Below by SEM photo, XRD figure spectrum and PL spectrum the structure of the ZnO nanometer stick array of the present invention's preparation and pattern and optical property are tested and characterized.
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates that load has the ZnO nanometer stick array of growing on the silicon chip matrix of ZnO film.As can be seen from Figure 1, the diffraction peak peak shape is sharp-pointed, good crystallinity, and the inclusion-free peak occurs, and can prove that product is hexagonal wurtzite structure.Peak-to-peak shape is sharp-pointed among the figure, the ZnO nanostructure has been described along c axle preferential growth, namely grows with the substrate vertical direction.Along with the increase of sodium-chlor doping content, move toward the Small angle direction gradually the diffraction peak position, and this is because the ratio of ionic radii Zn of Na big, and after Na replaced the position of Zn, spacing increased.
Synthetic ZnO nanometer stick array is carried out scanning electronic microscope (SEM) pattern characterize, shape appearance figure as shown in Figure 2.The nanometer rod of Hydrothermal Growth preparation is evenly gathered on silicon chip substrate, grows to arrange along the direction perpendicular to silicon chip substrate to form neat nanometer rod, and direction of growth unanimity, the size homogeneous, and also the top of each nanometer rod is smooth with the surface.Pure ZnO nanometer stick array diameter is 30 nm, and length is 750 nm.Along with the increase of sodium-chlor doping content, the nanometer one-dimensional array is more and more intensive, be close to be tiled in the silicon chip substrate surface fully, and because the shortening of length, the directivity of one-dimensional array is more excellent.The doping of sodium-chlor is 0.0409g, and when 0.0818g and 0.1227 g and 0.1636g, the diameter of nanometer rod is respectively 50 nm, 60 nm, and 70 nm and 70 nm, length is respectively 150 nm, 112 nm, 98 nm and 71 nm.As seen along with the increase of sodium-chlor doping content, the diameter of nanometer rod increases gradually, and length then reduces gradually.
Adopt spectrograph to carry out light at room temperature photoluminescence test under 325 nm laser synthetic ZnO nanometer stick array, gained light at room temperature photoluminescence collection of illustrative plates as shown in Figure 3.As seen from Figure 3, prepared ZnO nanometer stick array has a strong ultraviolet emission peak near 375 nm, and this mainly is because the compound generation of band-to-band transition of free exciton is the intrinsic emission peak of ZnO semiconductor material.Simultaneously can see except the ultraviolet emission peak, not having other assorted peaks again, illustrate that the sample surfaces defective that makes is less, the crystalline quality height.
Obviously, the above embodiment of the present invention only is for example of the present invention clearly is described, and is not to be restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here need not also can't give all embodiments exhaustive.All any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., all should be included within the protection domain of claim of the present invention.
Claims (9)
1. the preparation method of a Na doping zinc oxide nanometer rod array is characterized in that, may further comprise the steps:
S1. substrate is cleaned: substrate is successively with acetone, alcohol, deionized water ultrasonic cleaning and oven dry, standby;
S2. ZnO Seed Layer precursor solution preparation: a certain amount of zinc acetate and thanomin are joined in the ethylene glycol monomethyl ether successively, after fully stirring, make ZnO Seed Layer precursor solution after the sealing homogenizing;
S3. ZnO Seed Layer preparation: the substrate after will cleaning is transferred on the equal glue machine, drips ZnO Seed Layer precursor solution, is coated with after treating evenly to disperse, and anneal is carried out in the substrate that will be coated with ZnO Seed Layer precursor solution after the drying;
S4. the configuration of growth solution: hexamethylenetetramine, Zinc diacetate dihydrate and sodium-chlor are added in the deionized water, stir, obtain growth media;
S5. the preparation of ZnO nanometer stick array: the substrate that will contain the ZnO Seed Layer is immersed in the growth media, at 90 ℃ of growth 2～48 h down, and naturally cooling then, the rear film of will grow is rinsed the back drying well with deionized water, makes the ZnO nanometer stick array.
2. the preparation method of a kind of Na doping zinc oxide nanometer rod array according to claim 1 is characterized in that described substrate is silicon chip, sapphire, quartz or slide glass.
3. the preparation method of a kind of Na doping zinc oxide nanometer rod array according to claim 1 is characterized in that among the described step S2, the volumetric molar concentration of zinc acetate and thanomin is 75mM.
4. the preparation method of a kind of Na doping zinc oxide nanometer rod array according to claim 1 is characterized in that, among the described step S2, the time of sealing homogenizing is 24h.
5. the preparation method of a kind of Na doping zinc oxide nanometer rod array according to claim 1 is characterized in that, among the described step S3, the process that is coated with is for starting sol evenning machine, 500 rpm are coated with 20 s, are coated with 60 s with 5000 rpm again, 120 ℃ of following dry 15 min.
6. the preparation method of a kind of Na doping zinc oxide nanometer rod array according to claim 5 is characterized in that the described process repetitive operation that is coated with 4 times.
7. the preparation method of a kind of Na doping zinc oxide nanometer rod array according to claim 1 is characterized in that among the described step S3, anneal is in retort furnace, carries out anneal 2 h under 360 ℃.
8. the preparation method of a kind of Na doping zinc oxide nanometer rod array according to claim 1 is characterized in that among the described step S4, the volumetric molar concentration of hexamethylenetetramine and Zinc diacetate dihydrate is 12.5mM, and deionized water is 10ml.
9. the preparation method of a kind of Na doping zinc oxide nanometer rod array according to claim 1 is characterized in that among the described step S4, sodium-chlor is 0.0409 g or 0.0818 g or 0.1227 g or 0.1636 g.
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| CN103474574A (en) * | 2013-09-26 | 2013-12-25 | 天津理工大学 | Hybrid solar cell with aluminum-doped zinc oxide nanorod as electron transfer layer |
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| CN104926154A (en) * | 2015-06-08 | 2015-09-23 | 济南大学 | Self-cleaning heat-absorbing glass |
| CN105271362A (en) * | 2015-10-31 | 2016-01-27 | 合肥师范学院 | Preparation method of ZnO nano-structure with petal effect |
| CN107287615A (en) * | 2017-06-01 | 2017-10-24 | 北京科技大学 | A kind of vanadium doping ZnO nano-rod array light anode and its preparation method and application |
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| CN103474574A (en) * | 2013-09-26 | 2013-12-25 | 天津理工大学 | Hybrid solar cell with aluminum-doped zinc oxide nanorod as electron transfer layer |
| CN104634825A (en) * | 2015-01-28 | 2015-05-20 | 天津大学 | Preparation method of porous silicon-based tungsten oxide composite structural gas-sensitive element used at room temperature |
| CN104926154A (en) * | 2015-06-08 | 2015-09-23 | 济南大学 | Self-cleaning heat-absorbing glass |
| CN105271362A (en) * | 2015-10-31 | 2016-01-27 | 合肥师范学院 | Preparation method of ZnO nano-structure with petal effect |
| CN107287615B (en) * | 2017-06-01 | 2019-10-11 | 北京科技大学 | A kind of vanadium doping ZnO nano-rod array light anode and its preparation method and application |
| CN107287615A (en) * | 2017-06-01 | 2017-10-24 | 北京科技大学 | A kind of vanadium doping ZnO nano-rod array light anode and its preparation method and application |
| CN108130512A (en) * | 2017-11-21 | 2018-06-08 | 同济大学 | ZnO:Ga monocrystal nano rods array X radiographic flicker conversion screen and its preparation method and application |
| CN108918630A (en) * | 2018-05-16 | 2018-11-30 | 天津理工大学 | A kind of preparation method of Al doping ZnO ultrathin nanometer piece sensitive material and the purposes of gained nano sensitive material |
| CN109534285A (en) * | 2018-11-06 | 2019-03-29 | 浙江海洋大学 | A kind of ZnO nano column and preparation method based on photon structure seed layer |
| CN110211813A (en) * | 2019-06-25 | 2019-09-06 | 中原工学院 | Rodlike nickel hydroxide electrode material, preparation method and its supercapacitor of preparation |
| CN110211813B (en) * | 2019-06-25 | 2021-05-14 | 中原工学院 | Rod-shaped nickel hydroxide electrode material, preparation method and super capacitor prepared from rod-shaped nickel hydroxide electrode material |
| CN112275302A (en) * | 2020-10-26 | 2021-01-29 | 福州大学 | Preparation method of high-hydrophobicity iodine-doped ZnO composite film with antibacterial function |
| CN112275302B (en) * | 2020-10-26 | 2022-05-10 | 福州大学 | Preparation method of high-hydrophobicity iodine-doped ZnO composite film with antibacterial function |
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