CN1308244C - Nano zine oxide with excitating light strength and frequency tuning fluorescent frequency and it preparation - Google Patents
Nano zine oxide with excitating light strength and frequency tuning fluorescent frequency and it preparation Download PDFInfo
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- CN1308244C CN1308244C CNB2005100186105A CN200510018610A CN1308244C CN 1308244 C CN1308244 C CN 1308244C CN B2005100186105 A CNB2005100186105 A CN B2005100186105A CN 200510018610 A CN200510018610 A CN 200510018610A CN 1308244 C CN1308244 C CN 1308244C
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Abstract
The present invention relates to a nano-zinc oxide material with the effect on tuning fluorescent frequency by the intensity and the frequency of exciting light, and a preparation method thereof. The preparation method of the organic doped nano-zinc oxide material comprises: during the course of preparing common nano-zinc oxide with a hydrothermal method, adding organic materials of polyvinylpyrrolidone or PVA or polyethanediol, polyacrylamide, polyacrylic acid and polyepoxy ethane, cooling down to 65+/-5 DEG C to adjust and control the growth microscopic shape and the structure of nano-zinc oxide crystals. The prepared nano-zinc oxide material is spheroidal, ellipsoidal, rod-shaped, blossom-shaped or tubular, and has the characteristic of tuning fluorescence frequency effect by the intensity and the frequency of exciting light. When the material is excited by the exciting light, the frequency rule of radiation photons from a luminous center is changed with the intensity or the wavelength of the exciting light. The method has the advantages of simple method, easy industrialization, low energy consumption, no secondary pollution, low cost, stable performance, aging resistance, easy tuning realization and only two-nanon on-line property width of tuned fluorescence.
Description
Technical field
The present invention relates to material that has excitating light strength and frequency tuning fluorescence frequency effect and preparation method thereof, be specially nano zinc oxide material with excitating light strength and frequency tuning fluorescence frequency effect and preparation method thereof.
Background technology
Have the material of excitating light strength and frequency tuning fluorescence frequency effect, be mainly used in the series products such as laser apparatus, fiber amplifier, technique of display, photochemical catalysis and anti-counterfeiting technology, wide application prospect is arranged.Chinese by retrieval physics bibliographic data base, the scientific and technological achievement transaction data base, practical technique achievement database, Chinese patent database, CSTAD, china academia meeting paper database, Chinese Enterprise company and product database, the Sohu Advanced Search, CNKI knowledge innovation net, all places resource information net, the EI of national newspapers and periodicals index and international online retrieval DIALOG system, INSPEC, SCI, JICST, WILSON, APPL, AEROSPACE, CA, USPN, EP, YAHOO, NTIS database and related web site, the result does not have to find to have the nano zinc oxide material of excitating light strength and frequency tuning fluorescence frequency effect and any report and the introduction of technology of preparing thereof; Do not find any relevant report and practical application product with nano zinc oxide material product application of excitating light strength and frequency tuning fluorescence frequency effect yet.
Summary of the invention
The purpose of this invention is to provide a kind of nano material and preparation method thereof with excitating light strength and frequency tuning fluorescence frequency effect.
A kind of nano material with excitating light strength and frequency tuning fluorescence frequency effect that realizes goal of the invention is organic blended nano zine oxide.
Described organic blended thing is polyvinylpyrrolidone, polyvinyl alcohol, polyoxyethylene glycol, polyacrylamide, polyacrylic acid or polyethylene oxide.
The amount of described organic blended thing is the 2.5-10% of nano zine oxide quality.
Organic blended nano zine oxide of the present invention is shaped as sphere, elliposoidal, bar-shaped, flower-shaped or tubulose.
Preparation of nanomaterials with excitating light strength and frequency tuning fluorescence frequency effect of the present invention, it is characterized in that, zinc salt is dissolved in the water, in control pH=10 ± 0.5,100 ± 5 ℃ of temperature, under the agitation condition, in the common nano zinc oxide material process of Hydrothermal Preparation, add the organic inductive agent polyvinylpyrrolidone (PVP) or the polyvinyl alcohol (PVA) that advance prepared nano zine oxide quality 2.5-10%, polyoxyethylene glycol (PEG), polyacrylamide (PAM), polyacrylic acid (PAA) or polyethylene oxide (PEO), and reduce the temperature to 65 ± 5 ℃ and react, with regulation and control nano zine oxide crystal growth micro-shape and structure.
Test-results shows, with prescription of the present invention and the prepared nano zinc oxide material of preparation method can be sphere, elliposoidal, bar-shaped, flower-shaped, tubulose, and have excitating light strength and a frequency tuning fluorescence frequency performance characteristic, during with this material of excitation, energy (frequency) rule of luminescence center radiation photon with excitating light strength or wavelength change.
The present invention compared with prior art has following advantage and positively effect: material preparation method is simple, easily low, the non-secondary pollution of industrialized mass production, energy consumption, with low costly, tuning be easy to realize and by tuning fluorescence property excellence, live width only has about 2 nanometers.
Embodiment
Embodiment 1:
With zinc nitrate ((Zn (NO
3)
26H
2O) with the PEG of molecular weight 10000 and water by mass ratio=mix at 20: 1.5: 300, and place on the magnetic stirrer, add ammoniacal liquor during stirring and adjust pH value to 10, seal the glass mouth then, be warmed to 60 ℃ of continuously stirring 24 hours, last water cleaning and filtering three times is put into 60 ℃ of oven dry of baking oven and is promptly got required organic blendedly, and microcosmos geometric shape is the zinc oxide material of nano bar-shape.Its rod length is about 10 microns, and the diameter of rod is about 60 nanometers.The electron diffraction result is a single crystal.The experiment of the tuning fluorescence frequency effect of excitating light strength is carried out on the confocallaser microraman spectrometer of JY company at French LABRAM-HR.Experiment condition is a room temperature, and solid attitude powdered sample, excitation wavelength are He-Cd laser apparatus 325 nanometers.The result shows that excitating light strength is percent a period of time of green strength, and the fluorescence Spectra peak position is in 380 nanometers; Excitating light strength is green strength ten/one o'clock, and the fluorescence Spectra peak position is in 387 nanometers; Excitating light strength is that green strength four/for the moment, the fluorescence Spectra peak position is in 405 nanometers.The experiment of exciting light frequency tuning fluorescence frequency effect is carried out on the photoluminescence spectrometer at Edinburgh Instiments FLS-920.Experiment condition is a room temperature, and solid attitude powder is dispersed in sample in the ethanol, xenon source, and excitation wavelength is respectively 325,350,370 nanometers.The result shows, the fluorescence Spectra peak position is respectively 354,384,408 nanometers.
Embodiment 2: with zinc nitrate ((Zn (NO
3)
26H
2O) with the PEG of molecular weight 2000 and water by mass ratio=mix at 20: 1.5: 250, and place on the magnetic stirrer, add ammoniacal liquor adjustment pH value to 10 during stirring, seal the glass mouth then, be warmed to 60 ℃ of continuously stirring 24 hours.Last water cleaning and filtering three times is put into 60 ℃ of oven dry of baking oven and is promptly got required organic blendedly, and microcosmos geometric shape is nanotube-shaped zinc oxide material.Its pipe range is about 10 microns, and diameter is about 200 nanometers outside the pipe, and interior diameter is about 80 nanometers.The electron diffraction result is a single crystal.The experiment of the tuning fluorescence frequency effect of excitating light strength and experiment condition are with embodiment 1.The result shows that excitating light strength is percent a period of time of green strength, and the fluorescence Spectra peak position is in 380 nanometers; Excitating light strength is green strength ten/one o'clock, and the fluorescence Spectra peak position is in 390 nanometers; Excitating light strength is that green strength four/for the moment, the fluorescence Spectra peak position is in 415 nanometers.The experiments experiment of exciting light frequency tuning fluorescence frequency effect and experiment condition are with embodiment 1.The result shows, the fluorescence Spectra peak position is respectively 354,384,408 nanometers.
Example 3: with zinc nitrate ((Zn (NO
3)
26H
2O) with PVP and water by mass ratio=mix at 20: 1.5: 300, and place on the magnetic stirrer, add ammoniacal liquor during stirring and adjust pH value to 10, seal the glass mouth then, be warmed to 60 ℃ of continuously stirring 24 hours, last water cleaning and filtering three times is put into 65 ℃ of oven dry of baking oven and promptly get required organic blendedly, and microcosmos geometric shape is the flower-shaped zinc oxide material of nanometer rod composition.Its rod length is about 10 microns, and the diameter of rod is about 60 nanometers, and spending size is about 10 microns.The electron diffraction result is a single crystal.The experiments experiment of the tuning fluorescence frequency effect of excitating light strength and experiment condition are with embodiment 1.The result shows that excitating light strength is percent a period of time of green strength, and the fluorescence Spectra peak position is in 380 nanometers; Excitating light strength is green strength ten/one o'clock, and the fluorescence Spectra peak position is in 387 nanometers; Excitating light strength is that green strength four/for the moment, the fluorescence Spectra peak position is in 405 nanometers.The experiments experiment of exciting light frequency tuning fluorescence frequency effect and experiment condition are with embodiment 1.The result shows, the fluorescence Spectra peak position is respectively 354,384,408 nanometers.
Example 4: with zinc nitrate ((Zn (NO
3)
26H
2O) with PVA and water by mass ratio=mix at 20: 1.5: 250, and place on the magnetic stirrer, add ammoniacal liquor adjustment pH value to 10 during stirring, seal the glass mouth then, be warmed to 60 ℃ of continuously stirring 24 hours.Last water cleaning and filtering three times is put into 65 ℃ of oven dry of baking oven and promptly get required organic blendedly, and microcosmos geometric shape is the flower-shaped zinc oxide material of nanotube composition corn.Its pipe range is about 10 microns, and diameter is about 200 nanometers outside the pipe, and interior diameter is about 80 nanometers, and the popcorn size is about 10 microns.The electron diffraction result is a single crystal.The experiments experiment of the tuning fluorescence frequency effect of excitating light strength and experiment condition are with embodiment 1.The result shows that excitating light strength is percent a period of time of green strength, and the fluorescence Spectra peak position is in 380 nanometers; Excitating light strength is green strength ten/one o'clock, and the fluorescence Spectra peak position is in 390 nanometers; Excitating light strength is that green strength four/for the moment, the fluorescence Spectra peak position is in 415 nanometers.The experiments experiment of exciting light frequency tuning fluorescence frequency effect and experiment condition are with embodiment 1.The result shows, the fluorescence Spectra peak position is respectively 354,384,408 nanometers.
Example 5: with zinc nitrate ((Zn (NO
3)
26H
2O) with PAA and water by mass ratio=mix at 20: 2.0: 300, and place on the magnetic stirrer, add ammoniacal liquor adjustment pH value to 10 during stirring, seal the glass mouth then, be warmed to 60 ℃ of continuously stirring 24 hours.Last water cleaning and filtering three times is put into 65 ℃ of oven dry of baking oven and is promptly got required organic blendedly, and microcosmos geometric shape is that nanometer rod is formed axiolitic zinc oxide material.Its rod length is about 1.5 microns, and the diameter of rod is about 60 nanometers, forms about 1.5 microns of semimajor axis of ellipsoids, about 0.5 micron of minor semi-axis.The electron diffraction result is a single crystal.The experiments experiment of the tuning fluorescence frequency effect of excitating light strength and experiment condition are with embodiment 1.The result shows that excitating light strength is percent a period of time of green strength, and the fluorescence Spectra peak position is in 380 nanometers; Excitating light strength is green strength ten/one o'clock, and the fluorescence Spectra peak position is in 387 nanometers; Excitating light strength is that green strength four/for the moment, the fluorescence Spectra peak position is in 405 nanometers.The experiments experiment of exciting light frequency tuning fluorescence frequency effect and experiment condition are with embodiment 1.The result shows, the fluorescence Spectra peak position is respectively 354,384,408 nanometers.
Example 6: with zinc nitrate ((Zn (NO
3)
26H
2O) with PEO and water by mass ratio=mix at 20: 0.5: 250, and place on the magnetic stirrer, add ammoniacal liquor adjustment pH value to 10 during stirring, seal the glass mouth then, be warmed to 60 ℃ of continuously stirring 24 hours.Last water cleaning and filtering three times is put into 65 ℃ of oven dry of baking oven and is promptly got required organic blendedly, and microcosmos geometric shape is that nanometer rod is formed axiolitic zinc oxide material.Its rod length is about 1.5 microns, and the diameter of rod is about 60 nanometers, about 1.5 microns of semimajor axis of ellipsoids, about 0.5 micron of minor semi-axis.The electron diffraction result is a single crystal.The experiments experiment of the tuning fluorescence frequency effect of excitating light strength and experiment condition are with embodiment 1.The result shows that excitating light strength is percent a period of time of green strength, and the fluorescence Spectra peak position is in 380 nanometers; Excitating light strength is green strength ten/one o'clock, and the fluorescence Spectra peak position is in 390 nanometers; Excitating light strength is that green strength four/for the moment, the fluorescence Spectra peak position is in 415 nanometers.The experiments experiment of exciting light frequency tuning fluorescence frequency effect and experiment condition are with embodiment 1.The result shows, the fluorescence Spectra peak position is respectively 354,384,408 nanometers.
Claims (3)
1, a kind of nano material with excitating light strength and frequency tuning fluorescence frequency effect, it is characterized in that organic blended nano zine oxide, described organic blended hotchpotch is polyvinylpyrrolidone, polyvinyl alcohol, polyoxyethylene glycol, polyacrylamide, polyacrylic acid or polyethylene oxide, and the amount of described organic blended thing is the 2.5-10% of nano zine oxide quality.
2, nano material as claimed in claim 1 is characterized in that described organic blended nano zine oxide is shaped as sphere, elliposoidal, bar-shaped, flower-shaped or tubulose.
3, the described preparation of nanomaterials of claim 1 with excitating light strength and frequency tuning fluorescence frequency effect, it is characterized in that, zinc salt is dissolved in the water, in the hydrothermal method process of control pH=10 ± 0.5, agitation condition, add the polyvinylpyrrolidone, polyvinyl alcohol, polyoxyethylene glycol, polyacrylamide, polyacrylic acid or the polyethylene oxide that advance prepared nano zine oxide quality 2.5-10%, and under 65 ± 5 ℃ of temperature, react, with regulation and control nano zine oxide crystal growth micro-shape and structure.
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100391848C (en) * | 2006-03-02 | 2008-06-04 | 浙江大学 | Process for preparing zinc oxide nano stick |
| CN102951673B (en) * | 2012-11-29 | 2014-12-31 | 中国日用化学工业研究院 | Preparation method of nano zinc oxide rod |
| CN103043706B (en) * | 2012-12-04 | 2014-09-10 | 华南师范大学 | Preparation method of zinc oxide nanorod with strong blue-violet light after being excited |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1526644A (en) * | 2003-09-19 | 2004-09-08 | 中国科学院上海硅酸盐研究所 | Wet chemical process of preparing nano zinc oxide wire |
| EP1461290A1 (en) * | 2001-12-07 | 2004-09-29 | Sung Park | A METHOD FOR PREPARING ZnO NANOPOWDER |
| CN1533985A (en) * | 2003-03-31 | 2004-10-06 | 上海大学 | Preparation method of nano-grade zinc oxide powder |
| CN1598076A (en) * | 2004-07-23 | 2005-03-23 | 清华大学 | Process for growing zine oxide monocrystal by hot water method |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1461290A1 (en) * | 2001-12-07 | 2004-09-29 | Sung Park | A METHOD FOR PREPARING ZnO NANOPOWDER |
| CN1533985A (en) * | 2003-03-31 | 2004-10-06 | 上海大学 | Preparation method of nano-grade zinc oxide powder |
| CN1526644A (en) * | 2003-09-19 | 2004-09-08 | 中国科学院上海硅酸盐研究所 | Wet chemical process of preparing nano zinc oxide wire |
| CN1598076A (en) * | 2004-07-23 | 2005-03-23 | 清华大学 | Process for growing zine oxide monocrystal by hot water method |
Non-Patent Citations (4)
| Title |
|---|
| PEG辅助氧化锌纳米棒的水热法制备 陶新永、张孝彬、孔凡志、林森、程继鹏、黄宛真、李昱、刘芙、许国良，化学学报，第62卷第17期 2004 * |
| PEG辅助氧化锌纳米棒的水热法制备 陶新永、张孝彬、孔凡志、林森、程继鹏、黄宛真、李昱、刘芙、许国良，化学学报，第62卷第17期 2004;氧化锌晶体的研究进展 宋词、杭寅、徐军，人工晶体学报，第33卷第1期 2004;紫外光照射下ZnO超微粒子表面上的光反应 陈四海、任新民，感光科学与光化学，第14卷第1期 1996 * |
| 氧化锌晶体的研究进展 宋词、杭寅、徐军，人工晶体学报，第33卷第1期 2004 * |
| 紫外光照射下ZnO超微粒子表面上的光反应 陈四海、任新民，感光科学与光化学，第14卷第1期 1996 * |
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