CN1970683A - Zinc oxide nano sheet film materials with UV luminescent characteristics and method for preparing same - Google Patents
Zinc oxide nano sheet film materials with UV luminescent characteristics and method for preparing same Download PDFInfo
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- CN1970683A CN1970683A CN 200510122642 CN200510122642A CN1970683A CN 1970683 A CN1970683 A CN 1970683A CN 200510122642 CN200510122642 CN 200510122642 CN 200510122642 A CN200510122642 A CN 200510122642A CN 1970683 A CN1970683 A CN 1970683A
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Abstract
The invention discloses a zinc oxide nanometer film with ultraviolet luminous property and making method, which comprises the following steps: reacting 0.1mol/L zinc nitrate hexahydrate and 0.025-0.05mol/L dimethyl aminoboron alkyl under 70-80 deg.c for 2-4h; washing the substrate with film through water; drying to obtain the product; adopting monocrystalline silicon or metal or glass or ceramic or mica or quartz as substrate.
Description
Technical field the present invention relates to a kind of thin-film material and method for making, especially has Zinc oxide nano sheet film materials of UV luminescent characteristics and preparation method thereof.
Background technology metal oxide film, especially wide-band gap semiconductor thin film are having a wide range of applications aspect blue light and the ultraviolet photoelectron device.Zinc oxide is a kind of novel II～direct wide bandgap compound semiconductors material of VI family, have excellent optics and electrology characteristic, band gap under the room temperature is 3.37eV, exciton bind energy is 60meV, greater than the hot ionization energy (25meV) under the room temperature, possessed the supremacy clause of emission blue light or near-ultraviolet light, can develop multiple luminescent devices such as ultraviolet, blue light, green glow.Zinc oxide based semiconductor film photoelectric device mainly comprises ultraviolet detector, photodiode and semiconductor laser etc., can be widely used in fields such as optical communication network, photoelectric display, photoelectricity storage, photoelectricity conversion and photodetection, in addition, also can be used as transmitter, electrode of solar battery and top coat etc.People have done some trials and effort in order to obtain it, as a kind of " preparation method of strong uv-absorbing Nano zinc oxide film " who discloses among the disclosed Chinese invention patent ublic specification of application CN 1563485A on January 12nd, 2005.It is intended to provide a kind of has strong absorption and good to visible light permeability, simple to operate to UV-light, the preparation method of the Zinc oxide film material that temperature of reaction is low, cost is low, production efficiency is high; Wherein, zinc-oxide film is that the ball shaped nano Zinc oxide particles of 120 nanometers is formed by being covered in median size on the quartz substrate, the preparation method is at first being that zinc nitrate hexahydrate and six methylene radical four ammonia of 1: 1 are dissolved in the methanol solution respectively with the volumetric molar concentration ratio, be prepared into the film reaction soln, to immerse the vitriol oil, acetone then successively and immerse in the film reaction solution for preparing through the quartz substrate of supersound process, soak after 30～60 minutes, be warming up to 95～100 ℃ of reactions 2～3 hours again, take out after deionized water rinsing, dry and make thin-film material.But this preparation method exists weak point, and at first, the Zinc oxide film material of preparing only has the performance that absorbs UV-light and visible light transmissive, and does not have the performance of ultra-violet light-emitting; Secondly, the preparation method is numerous and diverse and the cycle is long, both need use methyl alcohol in reaction soln, substrate needs again to soak in the sulfuric acid of high density for a long time, and in acetone the supersound process of long period, the temperature of reacting required is also higher, causes production cost height, efficient low; Once more, the kind of the substrate that uses in the preparation is single, except that the preparation that is not easy to film, also makes the use range of thin-film material be subjected to certain restriction.
The summary of the invention the technical problem to be solved in the present invention provides a kind of widely applicable for overcoming weak point of the prior art, prepares the easy Zinc oxide nano sheet film materials of UV luminescent characteristics and preparation method thereof that has.
Zinc oxide nano sheet film materials with UV luminescent characteristics comprises the zinc-oxide film that is covered with single crystal structure on the substrate, particularly said film is made of nano-sheet zinc oxide, the planar dimension of said nanometer sheet is that 2～10 μ m, thickness are 30～80nm, and the thickness of said film is 2～20 μ m.
As the further improvement of the Zinc oxide nano sheet film materials with UV luminescent characteristics, described substrate is silicon single crystal or metal or glass or pottery or mica or quartz.
Preparation method with Zinc oxide nano sheet film materials of UV luminescent characteristics comprises liquid phase method, particularly it is finished according to the following steps: to place by concentration be the precursor solution that the zinc nitrate hexahydrate solution of 0.1 mol and dimethyl aminoboron alkyl solution that concentration is 0.025～0.05 mol are mixed with to the substrate that will clean earlier, in 70～80 ℃ of reactions 2～4 hours down; The substrate that will be covered with film again takes out the water flushing, makes the Zinc oxide nano sheet film materials with UV luminescent characteristics after the drying.
As the preparation method's of the Zinc oxide nano sheet film materials with UV luminescent characteristics further improvement, described substrate is silicon single crystal or metal or glass or pottery or mica or quartz; The scavenging solution of described monocrystalline substrate is for being that 2: 1 the vitriol oil and 30% hydrogen peroxide is formulated with volume ratio; Described water is deionized water or distilled water; Described exsiccant temperature is 50～80 ℃, and the time is 0.5～1.5 hour.
Beneficial effect with respect to prior art is, one, the thin-film material that makes is used field emission scanning electron microscope and transmission electron microscope and x-ray diffractometer respectively, the X-gamma spectrometer characterizes, from the stereoscan photograph that obtains, transmission electron microscope photo and corresponding selected area electron diffraction photo, and X-ray diffraction spectrogram, X-ray energy loss spectrogram as can be known, the thickness of film is 2～20 μ m, it is by numerous, the nanometer sheet accumulation that is basically perpendicular to substrate forms, the yardstick of nanometer sheet is 2～10 μ m, thickness is 30～80nm, the angle on its adjacent both sides is 120 degree, and some nanometer sheet wherein are hexagons of rule.Upper and lower two surfaces of nanometer sheet are very smooth, are that { the 0001} face has confirmed that it is the zinc oxide of single crystal structure.The monocrystalline hexagonal wurtzite structure that this single-crystal zinc-oxide nano sheet is a zinc oxide.The atom number per-cent of the zinc of film and oxygen element is near the desirable stoicheiometry of zinc oxide; They are two years old, to film respectively in the photoabsorption test of carrying out the ultraviolet-visible light district on the vitreous silica substrate with on any substrate, carry out the test of fluorescence, by test result as can be known, film has good light transmission at visible region, and ultraviolet (＜380nm) the light district has very strong absorption.Film has sent very strong UV-light under the exciting of excitation light source, its photoluminescent property has proved that film has good crystal mass, and in a word, film has excellent optical property; Its three, it is few and cheap and easy to get to prepare used raw material type, technological process is simple, the time is short, the temperature of reacting required is low, is easy to industrialized production; Its four, the kind of substrate is many, and film can be prepared on any substrate, has expanded the use range of film widely.
Description of drawings is described in further detail optimal way of the present invention below in conjunction with accompanying drawing.
Fig. 1 observes the stereoscan photograph that the back is taken to the thin-film material that makes with JEOL JSM-6700 F type and FEI Sirion 200 type field emission scanning electron microscopes, and the illustration in the photo is the partial enlarged drawing of scanning electron microscope.Fig. 1 a shows is that the concentration of the zinc nitrate hexahydrate solution in the precursor solution is the shape appearance figure of the film for preparing when being 0.05 mol of the concentration of 0.1 mol, dimethyl aminoboron alkyl solution, and Fig. 1 b shows is that the concentration of the zinc nitrate hexahydrate solution in the precursor solution is the shape appearance figure of the film for preparing when being 0.025 mol of the concentration of 0.1 mol, dimethyl aminoboron alkyl solution.Can be seen that by Fig. 1 a and Fig. 1 b the Zinc oxide particles that constitutes film all presents sheet, their typical sizes is 2～10 microns, and thickness is about 50 nanometers, shown in the illustration of Fig. 1 a upper left side.And the angle on the adjacent both sides of many sheet zinc oxides is 120 degree, shown in arrow in the illustration of Fig. 1 a upper right side.It is hexagons of rule that some oxidation zinc metal sheets are more arranged, shown in the illustration of Fig. 1 b lower right;
Fig. 2 be with the film in the thin-film material by ultrasonic transfer on the transmission electron microscope copper mesh after, with Japanese H-800 and JEOL-2010 type transmission electron microscope it is observed the transmission electron microscope photo that the back is taken, Fig. 2 a and Fig. 2 b show all is shape appearance figures of the film for preparing when being respectively 0.1 mol and 0.05 mol of the concentration of zinc nitrate hexahydrate in the precursor solution and dimethyl aminoboron alkyl, wherein, Fig. 2 a observes the photo of taking under the low power, the atomic lattice striped picture (high resolution photo) that Fig. 2 b takes for high power observation post, the illustration of Fig. 2 a and Fig. 2 b lower left all is corresponding selected area electron diffraction styles.Can see that from Fig. 2 a the contrast of whole Zinc oxide nano sheet is that these upper and lower two surfaces that these oxidation zinc metal sheets are described are very smooth uniformly, the selected area electron diffraction style shows that these oxidation zinc metal sheets are single crystal structure.The distance that Fig. 2 b then demonstrates adjacent two lattice fringes is in 0.28nm and the hexagonal wurtzite zinc oxide structure (0
10) spacing is identical, can judge that by its corresponding selected area electron diffraction style the upper and lower surface of these Zinc oxide nano sheets is { 0001} a face;
Fig. 3 is the X-ray diffracting spectrum (XRD) that obtains after the thin-film material that makes is tested with Philips X ' Pert type x-ray diffractometer, and wherein, ordinate zou is a relative intensity, and X-coordinate is 2 times of diffraction angle.The zinc nitrate hexahydrate in the used reaction precursor liquid solution of thin-film material shown in this XRD and the concentration of dimethyl aminoboron alkyl are respectively 0.1 mol and 0.05 mol.By XRD as can be known, (be the peak of band numeral in the bracket, number: 36-1451) fit like a glove, illustrate that the film that makes is the polycrystalline hexagonal wurtzite structure of zinc oxide by standard spectrum with Zinc oxide powder standard diffraction spectra for each diffraction peak (five peaks of bottom among the figure);
Fig. 4 is the X-ray energy loss spectrogram that obtains after thin-film material shown in Figure 3 is tested with Oxford Inca type X-gamma spectrometer, and wherein, ordinate zou is a relative intensity, and X-coordinate is an energy.Show among the figure except the signal of the silicon that comes from substrate, be 43%: 41% from the zinc of film and the atom number per-cent of oxygen element, the zinc-oxide film that this explanation obtains with solution method is near the desirable stoicheiometry of zinc oxide;
Fig. 5 tests resulting figure as a result with Cary5E type spectrograph to the photoabsorption in the ultraviolet-visible light district of the thin-film material that makes, and wherein, ordinate zou is a relative intensity, and X-coordinate is a wavelength.The used substrate of thin-film material is that the zinc nitrate hexahydrate in vitreous silica, the reaction precursor liquid solution and the concentration of dimethyl aminoboron alkyl are respectively 0.1 mol and 0.05 mol.By uv-visible absorption spectra figure as can be known, film has good light transmission at visible region, and has very strong absorption in ultraviolet (＜380 nanometer) light district, and this strong absorption is that the band-to-band transition from zinc oxide causes;
Fig. 6 is using excitation light source to be 2Kw/cm as 325nm, exciting power density
2The He-Cd laser device under the room temperature thin-film material shown in Figure 3 after irradiation excites, being tested resulting figure as a result to the fluorescence property of thin-film material, wherein, ordinate zou is a relative intensity, X-coordinate is a wavelength.Fluorescence spectrum after being excited by thin-film material as can be known, being positioned at the 380nm place has a very strong ultra-violet light-emitting peak and halfwidth to be about 120 milli electron-volts, and be positioned at 450～650nm scope an almost negligible visible glow peak is arranged, previous glow peak is the interband emission of zinc oxide semi-conductor, back one glow peak then be one relevant with deep energy level defect in the zincite crystal luminous.Hence one can see that, and thin-film material has good crystal mass.
Embodiment at first makes or buys from market silicon single crystal or metal or glass or pottery or mica or the quartz as substrate with ordinary method, and is placed in the scavenging solution and cleans up.Selecting for use by concrete substrate of scavenging solution determine, as to select silicon single crystal for use be substrate, and then its scavenging solution is for being that 2: 1 the vitriol oil and 30% hydrogen peroxide is formulated with volume ratio.
Embodiment 1: to place by concentration be the precursor solution that the zinc nitrate hexahydrate solution of 0.1 mol and dimethyl aminoboron alkyl solution that concentration is 0.025 mol are mixed with to the monocrystalline substrate that will clean earlier, in 70 ℃ of reactions 4 hours down.The substrate that will be covered with film again takes out uses deionized water rinsing, then in 50 ℃ dry 1.5 hours down, make as Fig. 1 b, be similar to Fig. 2 a and Fig. 2 b and as Fig. 3, Fig. 4, Fig. 6 be similar to the Zinc oxide nano sheet film materials shown in the curve among Fig. 5 with UV luminescent characteristics.
Embodiment 2: to place by concentration be the precursor solution that the zinc nitrate hexahydrate solution of 0.1 mol and dimethyl aminoboron alkyl solution that concentration is 0.032 mol are mixed with to the monocrystalline substrate that will clean earlier, in 73 ℃ of reactions 3.5 hours down.The substrate that will be covered with film again takes out uses distilled water flushing, then in 58 ℃ dry 1.3 hours down, make and be similar to Fig. 1 b, Fig. 2 a and Fig. 2 b and as Fig. 3, Fig. 4, Fig. 6 be similar to the Zinc oxide nano sheet film materials shown in the curve among Fig. 5 with UV luminescent characteristics.
Embodiment 3: to place by concentration be the precursor solution that the zinc nitrate hexahydrate solution of 0.1 mol and dimethyl aminoboron alkyl solution that concentration is 0.038 mol are mixed with to the monocrystalline substrate that will clean earlier, in 75 ℃ of reactions 3 hours down.The substrate that will be covered with film again takes out uses deionized water rinsing, then in 65 ℃ dry 1 hour down, make and be similar to Fig. 1 a, Fig. 2 a and Fig. 2 b and as Fig. 3, Fig. 4, Fig. 6 be similar to the Zinc oxide nano sheet film materials shown in the curve among Fig. 5 with UV luminescent characteristics.
Embodiment 4: to place by concentration be the precursor solution that the zinc nitrate hexahydrate solution of 0.1 mol and dimethyl aminoboron alkyl solution that concentration is 0.044 mol are mixed with to the monocrystalline substrate that will clean earlier, in 77 ℃ of reactions 2.5 hours down.The substrate that will be covered with film again takes out uses distilled water flushing, then in 73 ℃ dry 0.8 hour down, make and be similar to Fig. 1 a, Fig. 2 a and Fig. 2 b and as Fig. 3, Fig. 4, Fig. 6 be similar to the Zinc oxide nano sheet film materials shown in the curve among Fig. 5 with UV luminescent characteristics.
Embodiment 5: to place by concentration be the precursor solution that the zinc nitrate hexahydrate solution of 0.1 mol and dimethyl aminoboron alkyl solution that concentration is 0.05 mol are mixed with to the monocrystalline substrate that will clean earlier, in 80 ℃ of reactions 2 hours down.The substrate that will be covered with film again takes out uses deionized water rinsing, then in 80 ℃ dry 0.5 hour down, make as Fig. 1 a, Fig. 2 a and Fig. 2 b and as Fig. 3, Fig. 4, Fig. 6 be similar to the Zinc oxide nano sheet film materials shown in the curve among Fig. 5 with UV luminescent characteristics.
Select metal or glass or pottery or mica or quartz more respectively for use as substrate, repeat the foregoing description 1～5, make equally as or be similar to Fig. 1 a, Fig. 1 b, Fig. 2 a and Fig. 2 b and as Fig. 3, Fig. 4, Fig. 6 be similar to the Zinc oxide nano sheet film materials shown in the curve among Fig. 5 with UV luminescent characteristics.
Obviously, those skilled in the art can carry out various changes and modification to Zinc oxide nano sheet film materials with UV luminescent characteristics of the present invention and preparation method thereof and not break away from the spirit and scope of the present invention.Like this, if of the present invention these are revised and modification belongs within the scope of claim of the present invention and equivalent technologies thereof, then the present invention also is intended to comprise these changes and modification interior.
Claims (7)
1, a kind of Zinc oxide nano sheet film materials with UV luminescent characteristics, comprise the zinc-oxide film that is covered with single crystal structure on the substrate, it is characterized in that said film is made of nano-sheet zinc oxide, the planar dimension of said nanometer sheet is that 2～10 μ m, thickness are 30～80nm, and the thickness of said film is 2～20 μ m.
2, the Zinc oxide nano sheet film materials with UV luminescent characteristics according to claim 1 is characterized in that substrate is silicon single crystal or metal or glass or pottery or mica or quartz.
3, the preparation method with Zinc oxide nano sheet film materials of UV luminescent characteristics according to claim 1, comprise liquid phase method, it is characterized in that finishing according to the following steps: to place by concentration be the precursor solution that the zinc nitrate hexahydrate solution of 0.1 mol and dimethyl aminoboron alkyl solution that concentration is 0.025～0.05 mol are mixed with to the substrate that will clean earlier, in 70～80 ℃ of reactions 2～4 hours down; The substrate that will be covered with film again takes out the water flushing, makes the Zinc oxide nano sheet film materials with UV luminescent characteristics after the drying.
4, the preparation method with Zinc oxide nano sheet film materials of UV luminescent characteristics according to claim 3 is characterized in that substrate is silicon single crystal or metal or glass or pottery or mica or quartz.
5, the preparation method with Zinc oxide nano sheet film materials of UV luminescent characteristics according to claim 4, the scavenging solution that it is characterized in that monocrystalline substrate is for being that 2: 1 the vitriol oil and 30% hydrogen peroxide is formulated with volume ratio.
6 preparation methods with Zinc oxide nano sheet film materials of UV luminescent characteristics according to claim 3 is characterized in that water is deionized water or distilled water.
7, the preparation method with Zinc oxide nano sheet film materials of UV luminescent characteristics according to claim 3 is characterized in that the exsiccant temperature is 50～80 ℃, and the time is 0.5～1.5 hour.
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| CN101857222A (en) * | 2010-05-28 | 2010-10-13 | 常州大学 | Preparation method of large-area and continuous graphen/zinc oxide composite structure |
| CN102485680A (en) * | 2010-12-01 | 2012-06-06 | 北京信息科技大学 | Method for preparing a great amount of monocrystal zinc oxide nano rod arrays on glass by low temperature solution method |
| CN102757785A (en) * | 2011-04-26 | 2012-10-31 | 海洋王照明科技股份有限公司 | Luminescent film, preparation method thereof, and application thereof |
| CN103224215A (en) * | 2013-04-09 | 2013-07-31 | 中国科学院合肥物质科学研究院 | Hexagonal nanosheet array and preparation method thereof |
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| JP2004323818A (en) * | 2003-03-03 | 2004-11-18 | Japan Fine Ceramics Center | Luminescent material and light emitting device using the same |
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| CN100383923C (en) * | 2004-03-26 | 2008-04-23 | 北京大学 | Silicon substrate nano-zinc oxide and producing method and application thereof |
| CN1257311C (en) * | 2004-04-22 | 2006-05-24 | 上海交通大学 | Method for preparing nano zinc oxide film of high ultraviolet absorption |
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| CN101857222A (en) * | 2010-05-28 | 2010-10-13 | 常州大学 | Preparation method of large-area and continuous graphen/zinc oxide composite structure |
| CN102485680A (en) * | 2010-12-01 | 2012-06-06 | 北京信息科技大学 | Method for preparing a great amount of monocrystal zinc oxide nano rod arrays on glass by low temperature solution method |
| CN102757785A (en) * | 2011-04-26 | 2012-10-31 | 海洋王照明科技股份有限公司 | Luminescent film, preparation method thereof, and application thereof |
| CN102757785B (en) * | 2011-04-26 | 2014-01-08 | 海洋王照明科技股份有限公司 | Luminescent film, preparation method thereof, and application thereof |
| CN103224215A (en) * | 2013-04-09 | 2013-07-31 | 中国科学院合肥物质科学研究院 | Hexagonal nanosheet array and preparation method thereof |
| CN103224215B (en) * | 2013-04-09 | 2015-09-02 | 中国科学院合肥物质科学研究院 | Hexagonal nanosheet array and preparation method thereof |
| CN104445371A (en) * | 2014-11-25 | 2015-03-25 | 重庆文理学院 | Zinc oxide nanosheet material for photocatalysis and preparation method thereof |
| CN112142092A (en) * | 2019-06-26 | 2020-12-29 | 五邑大学 | ZnO nanosheet and preparation method thereof |
| WO2020258959A1 (en) * | 2019-06-26 | 2020-12-30 | 五邑大学 | Zno nanosheet and preparation method therefor |
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