CN101431148B - Method for improving illumination intensity of CdTe nano compound film - Google Patents
Method for improving illumination intensity of CdTe nano compound film Download PDFInfo
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- CN101431148B CN101431148B CN2008102010784A CN200810201078A CN101431148B CN 101431148 B CN101431148 B CN 101431148B CN 2008102010784 A CN2008102010784 A CN 2008102010784A CN 200810201078 A CN200810201078 A CN 200810201078A CN 101431148 B CN101431148 B CN 101431148B
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Abstract
The invention relates to a method which can improve the luminous intensity of a CdTe nano-composite thin film. NaHTe solution is firstly prepared by using sodium borohydride and tellurium powder withthe molar ratio of 1:1.7-2.0, then the NaHTe solution is added in mixed solution of CdCl2 and mercaptopropionic acid, the adding amount refers to that the molar ratio of CdCl2: NaHTe: mercaptopropionic acid is equal to 2:1:2-8, and the reflux is carried out at 50-110 DEG C for 5min-50h, thereby obtaining CdTe nanocrystal solution. Then, the polymerization of styrene monomers is carried out at 50-100 DEG C for 12-48h, so as to prepare polystyrene microspheres. PDDA polyelectrolyte solution and PSS polyelectrolyte solution with the concentration of 0.01-2.0mol/L and the pH of 6-12 are prepared.Finally, PDDA and PSS polyelectrolytes are repeatedly assembled on the polystyrene microspheres, CdTe nanocrystals and Zn<2+> with the same volume of 1 multiplied by 10<-10>-10mol/L are introduced into the reaction, thereby obtaining a layer of PS/PDDA/PSS/PDDA/CdTe fluorescent composite film by assembly; the operation of polyelectrolyte layer-nanocrystals is repeated to obtain the CdTe nano-composite thin film with the high luminous intensity. The method has simple process, low equipment requirement and low investment; compared with the pure CdTe nano-composite thin film, the luminous intensity is remarkably improved.
Description
Technical field
The present invention relates to a kind of method that can improve CdTe nano compound film luminous intensity.It specifically is doping of Zn in the CdTe nano compound film
2+Method.Doping of Zn with method preparation of the present invention
2+The CdTe nano compound film can improve in actual applications luminous intensity.
Background technology
CdTe is nanocrystalline to have that excitation spectrum is single, fluorescent line is narrow, luminous efficiency is high, glow color is adjustable, can carry out advantages such as polychrome combined mark.In addition, by changing the nanocrystalline size of CdTe, the nanocrystalline emission wavelength of CdTe can cover very big spectral region.These nanocrystalline advantageous properties of CdTe make it be with a wide range of applications at aspects such as biomedicine, photoelectric device, biology sensors.At present, the preparation of relevant CdTe semiconductor nano has many reports, as " preparation method of water-soluble CdTe nano crystal and preparation facilities thereof " (Chinese invention patent application number: 03127166.9, publication number: CN1524783) and " preparation method of the CdTe nano particle of water soluble and organic solvent " (the Chinese invention patent application number: 200710099085.3, publication number: CN101049918).CdTe is nanocrystalline fixing in some way or not only can improve nanocrystalline stability widely with film that other matrix complex group are dressed up nano-scale, and then realize the microcosmic of nanoparticle characteristic is regulated and control, but also can further expand its potential application at aspects such as electroluminescent device, display, biology sensors.Brilliant grade far away reported the static packaging technology of inducing with electric field in ITO (tin-doped indium oxide) substrate, prepared the CdTe that can be used for red and green electroluminescent device nanocrystalline/polyelectrolyte nano compound film (Journal of Nanoscience and Nanotechnology, 2001,1 (2): 133-136).Gan Lihua etc. reported a kind of CdTe of preparation nano compound film method (method for preparing polyelectrolyte/CdTe nano compound film, the Chinese invention patent application number: 200710041832.8, publication number: CN101085840).Improve the fluorescence intensity of the nanocrystalline or CdTe nano thin-film of CdTe, can further expand its application in practice.This method quality of forming film is more stable, but luminous intensity has much room for improvement.Up to now, also do not find technology simply to improve the method for CdTe nano compound film luminous intensity both at home and abroad, this makes its application produce a lot of problems.Therefore, the research of the method for exploration raising nano compound film luminous intensity has practical significance.
Summary of the invention
The objective of the invention is to be to disclose that a kind of technology is simple, steady quality, function admirable, the method for CdTe nano compound film luminous intensity of improving.The CdTe nano compound film of the doped metal ion of Huo Deing can overcome the common CdTe nano compound film not high shortcoming of luminous intensity in actual applications in this way, for the practical application of CdTe nano compound film in fields such as luminescent devices lays the first stone.
In order to achieve the above object, the present invention's doping of Zn in pure CdTe nano compound film
2+, prepared and contained Zn
2+The CdTe nano compound film.
Concrete preparation method carries out as follows:
The first step, the preparation of CdTe nanocrystalline colloidal sol
Measure sodium borohydride earlier: tellurium powder=1: the 1.7-2.0 mol ratio, then will sodium borohydride and the tellurium powder add in the reactor and react, reactor is with ice-cooled and reserve the hydrogen that outlet is discharged generation in the reaction.Behind reaction 2～8h, the tellurium powder disappears, and reactor bottom generates the sodium tetraborate precipitation of white, and the NaHTe solution that floats on the sodium tetraborate precipitation surface with in the reactor joins CdCl with microsyringe
2And in mercaptopropionic acid (MPA) mixed solution, under pH=7～14 and nitrogen protection, 50-110 ℃ of backflow 5min～50h promptly obtains the CdTe nanocrystal solution.
CdCl
2And the proportioning of mercaptopropionic acid (MPA) mixed solution is CdCl
2(: NaHTe: MPA=2: 1: 2～8 mol ratios.
Second step, the preparation of polystyrene microsphere
Measure PVP deionized water absolute ethyl alcohol=1: 3.8: 23.8 mass ratio, PVP, deionized water and absolute ethyl alcohol are joined in the 250mL three-necked bottle, after stirring forms homogeneous system, N
2Protection begins slowly to drip the styrene monomer of AIBN down after 0.5～5 hour, after dropwising, keep nitrogen atmosphere and mixing speed, at 50～100 ℃ of following polymerization reaction 12～48h, promptly gets polystyrene microsphere.
The 3rd step, the preparation of polyelectrolyte solution
Get PDDA and PSS stoste, the concentration that is dissolved in respectively with the high purity water preparation is 0.01～2.0molL
-1NaCl solution in, make PDDA and PSS polyelectrolyte solution that concentration is 0.1-20mg/L, the pH value of PDDA and PSS polyelectrolyte solution is all adjusted to 6～12.
In the 4th step, high luminous intensity CdTe receives the preparation of nano compound film
Earlier the polystyrene microsphere that second step was obtained cleans three times with cushioning liquid, and cleaning process comprises polystyrene microsphere sonic oscillation 5～50 minutes and centrifugal filtration 5～50 minutes each time; Carried out self assembly 5～50 minutes in the polystyrene microsphere that the PDDA polyelectrolyte solution adding in the 3rd step was cleaned again.Clean secondary with cushioning liquid again; Then carry out the PSS self assembly, clean twice with cushioning liquid equally again according to identical program.Repeat again at last the PDDA assembling process once after, CdTe nanocrystal solution that the first step is obtained and reaction environment are with 1 * 10 of volume
-10The Zn of～10mol/L
2+(from the pure ZnCl of analysis of Chinese Medicine (group) chemical reagent Co., Ltd purchase
2Crystal) adds, reacted 5～50 minutes, clean secondary, so just obtained one deck PS/PDDA/PSS/PDDA/CdTe composite fluorescent film with cushioning liquid.Repeat above polyelectrolyte layer-nanocrystalline operation, just can obtain the high luminous intensity CdTe nano compound film of the number of plies of designing requirement.
The present invention has the following advantages:
1. the present invention has selected doping of Zn in the CdTe nano compound film
2+, pass through Zn
2+, CdTe is nanocrystalline and the matrix of having assembled polyelectrolyte reacts jointly, prepared and contained Zn
2+The CdTe nano compound film.Its operating procedure is simple, condition is controlled easily, equipment requirements is low, with low cost.
2. the product of the CdTe nano compound film that makes of the inventive method are of fine quality, the analysis showed that after tested, and the spectrum of gained film shows and impurity peaks do not occur, fluorescence peak half-peak width proves that particle size is even, and has good stability, nanocrystalline on film marshalling, thickness is even.
3. the present invention's doping of Zn in CdTe nano compound film preparation process
2+, do not need to add any other additive, so environmentally safe and technology are reliable.
4. because the present invention adopts mercaptopropionic acid is that stabilizer package overlays on the CdTe nanocrystal surface and makes that CdTe is nanocrystalline and have a core/shell structure, simultaneously, because its coating makes the CdTe nanocrystal surface electronegative, thereby stoped the reunion of CdTe between nanocrystalline effectively, improved the stability of CdTe nano compound film greatly.
5. by doping of Zn in the CdTe nano compound film
2+The doping of Zn that makes
2+The CdTe nano compound film, detect through spectrum contrast, the luminous intensity of sample is about 950, half-peak breadth is about 45nm, the characteristic peak wavelength is about 600nm; And be about 250, half-peak breadth and characteristic peak positions and doping of Zn with the luminous intensity of the pure CdTe nano compound film sample of concentration
2+CdTe nano compound film sample situation approaching.So with pure Zn
2+The CdTe nano compound film compare doping of Zn
2+After the luminous intensity and the luminous efficiency of the CdTe nano compound film that makes be significantly improved.
Description of drawings
The fluorescence spectrum figure of the CdTe nano compound film that Fig. 1 makes for the inventive method
Embodiment
Embodiment 1
In the 10mL centrifuge tube, add the sodium borohydride 80mg of commercially available SILVER REAGENT, the 1mL high purity water reinjects.Add the 134.85mg tellurium powder of commercially available SILVER REAGENT then, the external application of 10mL centrifuge tube is ice-cooled, and centrifuge tube seals and insert a syringe needle to discharge the hydrogen that produces in the reaction with rubber stopper.Behind the 2h, the tellurium powder disappears, and generates the sodium tetraborate precipitation of white at the bottom of the centrifuge tube.Solution is NaHTe solution in the centrifuge tube, and NaHTe solution is isolated, and is standby.The NaHTe solution that above-mentioned separation is obtained joins 1.25 * 10 with microsyringe
-3The CdCl of mol/L
2And in mercaptopropionic acid (MPA) mixed solution, regulate pH=14 with 1mol/L NaOH, nitrogen protection promptly obtained the CdTe nanocrystal solution in 50 hours 110 ℃ of backflows.
CdCl
2And the proportioning of mercaptopropionic acid (MPA) mixed solution is CdCl
2(: NaHTe: MPA=2: 1: 2 mol ratio.NaHTe and MPA are commercial reagent level raw materials.
PVP, 7.6mL deionized water and the 60.4mL absolute ethyl alcohol of 2g are joined in the 250mL three-necked bottle, after stirring forms homogeneous system, feed N
2Emptying, beginning slowly drips the 30.0g styrene monomer of 0.3gAIBN after 0.5 hour, after dropwising, keeps nitrogen atmosphere and stirring condition, at 50 ℃ of following polymerization reaction 48h, promptly gets polystyrene microsphere.
Get the pure PDDA of commercially available analysis of 0.5ml and PSS stoste (they are the solution of 20% mass concentration bought from Aldrich) and be dissolved in the polyelectrolyte solution of making PDDA and PSS the NaCl solution with the 0.01mol/L of high purity water preparation respectively, the concentration of polyelectrolyte solution is 0.1mg/L (calculating with monomer), with watery hydrochloric acid its pH value is transferred to 12.
Earlier with 0.5ml polystyrene microsphere 0.5ml, the cushioning liquid of pH=6.884 cleans three times, and cleaning process comprises polystyrene microsphere sonic oscillation 50 minutes and centrifugal filtration 50 minutes each time; Again the above-mentioned PDDA polyelectrolyte solution of 0.5ml is added polystyrene microsphere and carried out self assembly 50 minutes, clean secondary; Identical process cleans twice with the self assembly of 0.5ml PSS polyelectrolyte solution again; Repeat again the PDDA self assembling process once after, the 1ml CdTe nanocrystal solution that will prepare at last and with Zn with the 10mol/L of volume
2+Introduce reaction 50 minutes, clean secondary, so just obtained one deck PS/PDDA/PSS/PDDA/CdTe composite fluorescent film.Repeat above operation and just can obtain multi-layer C dTe self assembly laminated film, this multi-layer C dTe self assembly laminated film is a high luminous intensity CdTe nano compound film.
The mol ratio of adjusting sodium borohydride and tellurium powder is 2: 1.Add the 40mg sodium borohydride in the 10mL centrifuge tube, the 1mL high purity water that reinjects adds 67.425mg tellurium powder then, and reaction system is with ice-cooled, and centrifuge tube seals and insert a syringe needle to discharge the hydrogen that produces in the reaction with rubber stopper.Behind the 8h, the tellurium powder disappears, and the bottle end generates the sodium tetraborate precipitation of white, and NaHTe solution floats on the surface of sodium tetraborate, and NaHTe solution is separated with sodium tetraborate, and is standby.PH=7 (adjusting of 1mol/L NaOH), nitrogen protection adds 0.63 * 10 with the NaHTe solution that newly makes with microsyringe
-3The CdCl of mol/L
2And in mercaptopropionic acid (MPA) mixed solution, promptly obtain the CdTe nanocrystal solution at 50 ℃ of backflow 5min.CdCl
2And the proportioning of mercaptopropionic acid (MPA) mixed solution is CdCl
2 (: NaHTe: MPA=2: 1: 8 mol ratio.
PVP, 3.8mL deionized water and the 30.2mL absolute ethyl alcohol of 1g are joined in the 250mL three-necked bottle, after stirring forms homogeneous system, feed N
2Emptying, beginning slowly drips the 15.0g styrene monomer of 0.15gAIBN after 5 hours, after dropwising, keeps nitrogen atmosphere and stirring, at 100 ℃ of following polymerization reaction 12h, promptly gets polystyrene microsphere.
The PDDA and the PSS stoste of getting 0.5mL are dissolved in the NaCl solution of the 2mol/L for preparing with high purity water, and its concentration is about 20mg/L, with watery hydrochloric acid its pH value is transferred to 6, makes PDDA and PSS polyelectrolyte solution.
Earlier the cushioning liquid of 0.5ml polystyrene microsphere with 0.5ml pH=6.884 is cleaned three times, cleaning process comprises polystyrene microsphere sonic oscillation 5 minutes and centrifugal filtration 5 minutes each time; Again the 0.5ml PDDA polyelectrolyte solution for preparing is added polystyrene microsphere and carried out self assembly 5 minutes, clean secondary; Then 0.5ml PSS self assembling process cleans twice equally again; Repeat the PDDA process once after, the 1ml CdTe nanocrystal solution that will prepare at last and with reaction environment with 1 * 10 of volume
-10The Zn of mol/L
2+Introduce, reacted 5 minutes, clean secondary, so just obtained one deck PS/PDDA/PSS/PDDA/CdTe composite fluorescent film.Repeat above operation and just can obtain multi-layer C dTe self assembly laminated film.
This laminated film fluorescence spectrum sees that Fig. 1 (contains Zn
2+Concentration is 1 * 10
-5, 1 * 10
-4, 1 * 10
-3, 1 * 10
-2, 1 * 10
-1The fluorescence spectrum figure of mol/L and blank self-assembled film), increase with the Zn ion concentration as seen from the figure, fluorescence intensity increases thereupon, is 1 * 10 to concentration
-3During mol/L, fluorescence intensity reaches maximum, and when concentration strengthens again, fluorescence intensity descends rapidly, but still big when not adding the Zn ion.Proof Zn
2+Fluorescence intensity for film has humidification, and optium concentration is 1 * 10
-3Mol/L.
Claims (1)
1. method that improves CdTe nano compound film luminous intensity is characterized in that:
The first step, the preparation of CdTe nanocrystalline colloidal sol
Measure sodium borohydride earlier: tellurium powder=1: the 1.7-2.0 mol ratio, then will sodium borohydride and the tellurium powder add in the reactor and react, the reactor external application is ice-cooled and reserve outlet and discharge the hydrogen that produces in the reaction; Behind reaction 2～8h, the tellurium powder disappears, and the reactor inner bottom part generates white sodium tetraborate precipitation, with the NaHTe solution that floats on the sodium tetraborate precipitation surface in the reactor, is moved into CdCl with microsyringe
2In the mercaptopropionic acid mixed solution, under pH=7～14 and nitrogen protection, 50-110 ℃ of backflow 5min～50h promptly obtains the CdTe nanocrystal solution; CdCl
2With the proportioning of mercaptopropionic acid mixed solution and NaHTe solution be CdCl
2: NaHTe: mercaptopropionic acid=2: 1: 2～8 mol ratios;
Second step, the preparation of polystyrene microsphere
Measure PVP: deionized water: absolute ethyl alcohol=1: 3.8: 23.8 mass ratio, PVP, deionized water and absolute ethyl alcohol are joined in the three-necked bottle, after stirring forms homogeneous system, N
2Protection begins slowly to drip the styrene monomer of AIBN down after 0.5～5 hour, after dropwising, keep nitrogen atmosphere and mixing speed, at 50～100 ℃ of following polymerization reaction 12～48h, promptly gets polystyrene microsphere;
The 3rd step, the preparation of polyelectrolyte solution
Getting the concentration that PDDA and PSS stoste is dissolved in respectively with high purity water preparation is 0.01～2.0molL
-1NaCl solution in, make PDDA and PSS polyelectrolyte solution that concentration is 0.1-20mg/L, the pH value of PDDA and PSS polyelectrolyte solution is all adjusted to 6～12;
The 4th step, the preparation of high luminous intensity CdTe nano compound film
Earlier the polystyrene microsphere that second step was obtained cleans three times with cushioning liquid, and cleaning process comprises microballoon sonic oscillation 5～50 minutes and centrifugal filtration 5～50 minutes each time; Carry out self assembly 5～50 minutes in the PDDA polyelectrolyte solution adding polystyrene microsphere with the 3rd step again, clean secondary with cushioning liquid again; Then carry out the PSS self assembly, clean twice with cushioning liquid equally again according to identical program; Last repeat again the PDDA assembling process once the back add CdTe nanocrystal solution that the first step makes with 1 * 10 of volume
-10The Zn of～10mol/L
2+, reacted 5～50 minutes, clean secondary with cushioning liquid, obtained one deck PS/PDDA/PSS/PDDA/CdTe composite fluorescent film; Repeat above polyelectrolyte layer-nanocrystalline operation, obtain high luminous intensity CdTe nano compound film.
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| CN102991048B (en) * | 2012-10-18 | 2016-01-06 | 东华大学 | Electrostatic self-assembled method prepares schemochrome laminated film |
| CN104677946A (en) * | 2015-03-05 | 2015-06-03 | 浙江大学 | Graphene/titanium dioxide thin film gas sensor and preparation method thereof |
| CN105348550B (en) * | 2015-11-20 | 2018-07-06 | 西安交通大学 | A kind of preparation method of the PDMS film with temperature-sensing property |
| CN106959289B (en) * | 2017-03-22 | 2019-07-12 | 东南大学 | A kind of electrogenerated chemiluminescence material, preparation method and application |
| CN111239088A (en) * | 2020-01-17 | 2020-06-05 | 中山大学 | Micro-nano composite structure with fluorescence enhancement and optical amplification effects and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1524783A (en) * | 2003-09-18 | 2004-09-01 | 吉林大学 | Method and apparatus for preparing water-soluble CdTe nanocrystalline |
| US6855202B2 (en) * | 2001-11-30 | 2005-02-15 | The Regents Of The University Of California | Shaped nanocrystal particles and methods for making the same |
| CN101049918A (en) * | 2007-05-11 | 2007-10-10 | 北京化工大学 | Method for preparing CdTe Nano grains possible to be dissolved in water and organic solvent |
| CN101085840A (en) * | 2007-06-11 | 2007-12-12 | 同济大学 | Method for preparing polyelectrolyte/CdTe nano composite thin film |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6855202B2 (en) * | 2001-11-30 | 2005-02-15 | The Regents Of The University Of California | Shaped nanocrystal particles and methods for making the same |
| CN1524783A (en) * | 2003-09-18 | 2004-09-01 | 吉林大学 | Method and apparatus for preparing water-soluble CdTe nanocrystalline |
| CN101049918A (en) * | 2007-05-11 | 2007-10-10 | 北京化工大学 | Method for preparing CdTe Nano grains possible to be dissolved in water and organic solvent |
| CN101085840A (en) * | 2007-06-11 | 2007-12-12 | 同济大学 | Method for preparing polyelectrolyte/CdTe nano composite thin film |
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