CN102634338A - Preparing method of tunable photoluminescence polymer solid thin film - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000007787 solid Substances 0.000 title claims abstract description 24
- 229920000642 polymer Polymers 0.000 title claims abstract description 18
- 238000005424 photoluminescence Methods 0.000 title claims abstract description 11
- 239000010409 thin film Substances 0.000 title abstract 4
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 39
- 239000002105 nanoparticle Substances 0.000 claims abstract description 29
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 238000000502 dialysis Methods 0.000 claims abstract description 10
- 239000012530 fluid Substances 0.000 claims abstract description 5
- 229920000620 organic polymer Polymers 0.000 claims abstract description 5
- 239000012141 concentrate Substances 0.000 claims abstract description 3
- 238000002360 preparation method Methods 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 15
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 13
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 13
- 238000005530 etching Methods 0.000 claims description 8
- 230000003287 optical effect Effects 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 230000005284 excitation Effects 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 230000010355 oscillation Effects 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 230000001476 alcoholic effect Effects 0.000 claims description 4
- 238000005260 corrosion Methods 0.000 claims description 4
- 230000007797 corrosion Effects 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000000103 photoluminescence spectrum Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- QPJSUIGXIBEQAC-UHFFFAOYSA-N n-(2,4-dichloro-5-propan-2-yloxyphenyl)acetamide Chemical compound CC(C)OC1=CC(NC(C)=O)=C(Cl)C=C1Cl QPJSUIGXIBEQAC-UHFFFAOYSA-N 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
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- -1 carbon ion Chemical class 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
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Abstract
The invention provides a preparing method of a tunable photoluminescence polymer solid thin film. The preparing method comprises the following steps of: adding water suspending liquid of 3C-SiC nano-particle into mixed solution of crylic acid and ethanol, sequentially irradiating under the blue light and the ultraviolet light of 360nm for 1+/-0.3 hours, packing a layer of polyacrylic acid organic polymer on the surface of the nano-particle, putting reacted solution in a dialysis bag to wash out unreacted crylic acid and ethanol, and putting in 60+/-10 DEG C oven to concentrate for hours, so that yellow or brown transparent colloidal liquid can be obtained; and dropping the viscous fluid on a flat plate to be continuously dried, so that the silicon carbide nano-particle-packed polymer solid thin film can be obtained. The polymer solid thin film generated by the preparing method is compact and stable, so that the stable and tunable photoluminescence can be realized.
Description
Technical field
The present invention relates to a kind of method for preparing the polymer solids film that produces the tunable optical photoluminescence; Especially utilize vinylformic acid parcel 3C-SiC preparation of nanoparticles to generate method fine and close, the stable polymer solid film, this film can be realized stable tunable pl-.
Background technology
Silit is the third generation wide bandgap semiconductor materials that first elemental semiconductors (Si) and s-generation compound semiconductor materials GaAs, GaP and InP grow up afterwards.Silit not only has bigger band gap width (3C, 4H, 6H type silit band gap width at room temperature are respectively 2.24,3.22,2.86 eV); And have characteristics such as high critical breakdown electric field, high heat conductance, high carrier drift velocity, have huge application potential at aspects such as high temperature, high frequency, high-power, photoelectron and radioprotectives.Replace silicon with silit, preparation photoelectric device and unicircuit can be the raising of military electronic system and weaponry performance, and the electronics of anti-adverse environment provide new device.
For panchromatic demonstration, the blue light composition that is absolutely necessary again.Though 3C-SiC (SIC of cube solid matter) has bigger band gap width (2.24 eV); But its light-emitting zone is still in the scope of green glow; And because silit is a kind of indirect band-gap semiconductor material, the carbofrax material of body material luminous ten minutes at room temperature is faint.According to the quantum limitation effect correlation theory; Small-size effect can cause exciting with composite efficiency and strengthens greatly; So when the particle size of silit is reduced to nanometer scale, luminous efficiency will be greatly improved, be reduced to Bohr's exciton radius of body material when following when size simultaneously; The band gap of nano particle will be widened, thereby it luminously will reduce and blue shift takes place with particle size.So prepare undersized silicon-carbide particle, can realize its strong blue emission, this will produce material impact to microelectronics and optoelectronic areas.In addition, silit has goodish bio-compatibility, particularly with the compatibility of blood; And the density of SiC is less; Chemicalstability is better, thus the nanometer silicon carbide particle be expected to be used widely at biomedical sector, as can be as the luminous organism label etc.
In recent years, various devices with mixed structure of organic and inorganic nano material have obtained extensive studies, for example light emitting diode (LED), bistable state memory device and solar cell or the like.Wherein, the photo luminescent devices with organic and inorganic mixed structure based on colloid semi-conductor (like CdSe, ZnSe, ZnS etc.) nano particle becomes the LED hot research fields.Than traditional LED and OLED device, it has low cost, high brightness, saturated, the luminous plurality of advantages such as reaching colour tunable of stablizing of color.These characteristics make that such device is hopeful to be widely used in FPD and lighting field.Yet, rarely have report based on the electroluminescent device of SiC nano particle always.Main difficulty is SiC, and that works prepares nano particle with the method for chemosynthesis unlike other several kinds of semiconductor materials (like CdSe, ZnSe, ZnS etc.).
Nanometer silicon carbide particulate preparation in the past is main to be realized through two kinds of methods.First method is to generate the nanometer silicon carbide particle through various chemical reactions, injects silicon chip [L. S. Liao, X. M. Bao, Z. F. Yang, and N. B. Min, Appl. Phys. Lett. such as carbon ion
66, 2382 (1995)], carbon ion and silicon ion cosputtering silica membrane [J. Zhao, D. S. Mao, Z. X. Lin, B. Y. Jiang, Y. H. Yu, X. H. Liu, H. Z. Wang, and G. Q. Yang, Appl. Phys. Lett.
73, 1838 (1998)], C
60Coupling porous silicon [X. L. Wu, G. G. Siu, M. J. Stokes, D. L. Fan, Y. Gu, and X. M. Bao, Appl. Phys. Lett.
77, 1292 (2000)] etc. preparation method but these methods all can not prepare the nano particle of single structure phase, stable strong blue emission.Another kind method is an electrochemical erosion method, promptly uses the electrochemical process method, corrosion 3C-SiC polycrystalline sheet; Through sonic oscillation, obtain being suspended in the nanometer silicon carbide particle of solution again, can stablize the higher blue light of emissive porwer [X. L. Wu; J. Y. Fan, T. Qiu, X. Yang; G. Siu, and P. K. Chu, Phys. Rev. Lett.
94, 026102 (2005)], but this method prepares the process relative complex, the more important thing is, SiC polycrystalline sheet not only costs an arm and a leg, and preparation with purchase all difficult.
Nano particle is because its size is little, and structure and character are all quite complicated, and its surface state and defect state all have very big influence to its luminosity, and this makes has also just had very big difficulty to the luminous very difficult control of 3C-SiC nano particle on using.
Summary of the invention
This provides a kind of vinylformic acid parcel 3C-SiC preparation of nanoparticles of utilizing to generate method fine and close, the stable polymer solid film, and this film can be realized stable tunable pl-.
Technical scheme of the present invention: a kind of vinylformic acid that utilizes wraps up the method that the 3C-SiC preparation of nanoparticles produces the polymer solids film of tunable optical photoluminescence: the suspension-s of 3C-SiC nano particle in water is added in vinylformic acid and the alcoholic acid mixing solutions successively under blue light (490 nm) and UV-light (360 nm), carried out irradiation 1 ± 0.3 hour; Superscribe one deck ROHM organic polymer at nano grain surface; Place dialysis tubing to clean out unreacted vinylformic acid and ethanol reacted solution; And place 60 ± 10 ℃ of baking ovens to concentrate several hours, obtain yellow or brown transparent colloidal liquid.Above-mentioned viscous fluid is dripped to flat board (silicon chip etc.) continue drying, can obtain the polymer solids film of packaged silicon carbide nano particle.Above-mentioned solid film can obtain the photoluminescence spectrum of very strong luminous peak position with excitation wavelength adjustable (400 nm to 550 nm).
The 3C-SiC nano particle adopts the chemical corrosion method preparation: generally, micron-sized 3C-SiC powder is positioned over beaker as etch reactants, and etching solution is 65 wt% nitric acid (HNO
3) and 40 wt% hydrofluoric acid (HF) composition, the volume ratio of nitric acid and hydrofluoric acid is 1:3, and the quality of etching solution is more than six times of 3C-SiC powder, and the etching reaction temperature is 100 ± 10 ° of C, and the reaction times is 1 ± 0.2 hour.After the reaction, the mixed liquid of gained acid and powder is cooled to room temperature, left standstill several hours or centrifugation after, skim the upper strata and react remaining acid solution, the powder that obtains is cleaned the back oven dry repeatedly with deionized water.Powder after the oven dry is positioned in the glass beaker, adds deionized water, about 30～60 minutes of sonic oscillation, with products therefrom left standstill several hours or centrifugation after, get supernatant liquid, get final product the suspension-s of 3C-SiC nano particle in water.
With the suspension-s of the above-mentioned nanometer silicon carbide particle of 2-10 milliliter in water, add 2 milliliters of vinylformic acid and 20 milliliters of alcoholic acid mixing solutionss, sonic oscillation mixed it in 10 minutes; Removing wherein dissolved oxygen, the back was at blue light (490 nm) and UV-light (360 nm) difference irradiation 1 ± 0.3 hour down with the logical nitrogen of this mixed solution 30 minutes.It is 3500 dialysis tubing good seal that irradiated mixing solutions is injected molecular weight cut-off; Dialysis tubing inserted in the de-ionized water-bath isolated unreacted vinylformic acid and ethanol in several hours; After from dialysis tubing, pour into solution in the beaker; And place 60 ℃ of baking oven numbers hour, obtain yellow or brown transparent colloidal liquid.Above-mentioned viscous fluid is dripped to dull and stereotyped going up continue oven dry, can obtain the polymer solids film of packaged silicon carbide nano particle.
Beneficial effect of the present invention is following:
1. preparation method of the present invention is simple, need not complicated experimental installation, and experiment material is cheap and easy to be obtained;
2. the polymer solids film that generates is fine and close, stable, can realize stable to nano particle light emitting control so that obtain tunable pl-.And make things convenient for the widespread use of this type of material.
Description of drawings
Fig. 1. the transmission electron microscope photo (a) and the size distribution plot of the 3C-SiC nano particle that the present invention is used.Wherein (b) figure is (a) high resolution picture; (c) figure is the distribution of sizes of nano particle in the transmission electron microscope pictures taken.Can know that by figure its median size is 3.4 nm.
Fig. 2. the photoluminescence spectrum of the organic polymer solid film of the packaged silicon carbide nano particle that the present invention obtains.Excitation wavelength is selected 300nm to 500nm, whenever measures once at a distance from 20nm, obtains very strong with adjustable blue light to the green glow of excitation wavelength (450 nm to 550 nm) pl-peak, as shown in the figure.
Embodiment
Utilize vinylformic acid parcel 3C-SiC preparation of nanoparticles to produce the polymer solids film of tunable optical photoluminescence.
The 3C-SiC nano particle adopts the chemical corrosion method preparation: generally, the micron-sized 3C-SiC powder of about 6.0 grams is positioned over plastic beaker as reactant, and etching solution is 15 milliliter of 65 wt% nitric acid (HNO
3) and 45 milliliter of 40 wt% hydrofluoric acid (HF) composition, the etching reaction temperature is 100 ° of C, the reaction times is 1 hour.After the reaction, the mixed liquid of gained acid and powder is cooled to room temperature, left standstill several hours or centrifugation (8000 rev/mins, centrifugal 5 minutes) after, go to the upper strata to react remaining acid solution.The powder that obtains is cleaned with deionized water repeatedly, place baking oven under 70 ° of C, to dry in the powder that obtains again through several hours.Powder after the oven dry is positioned in the glass beaker, adds 30 ml deionized water, about 30～60 minutes of sonic oscillation.With products therefrom left standstill several hours or centrifugation (8000 rev/mins, centrifugal 10 minutes) after, get supernatant liquid, get final product the suspension-s of 3C-SiC nano particle in water.The transmission electron microscope characterization result shows that the nanocrystalline pattern of gained is an almost spherical, and obtaining size-grade distribution through the particle-size analyzer test is 1.5～6.5 nm.
With the suspension-s of the above-mentioned nanometer silicon carbide particle of 2-10 milliliter in water, add 2 milliliters of vinylformic acid and 20 milliliters of alcoholic acid mixing solutionss, sonic oscillation mixed it in 10 minutes; Removing wherein dissolved oxygen, the back was at blue light (490 nm) and UV-light (360 nm) difference irradiation 1 hour down with the logical nitrogen of this mixed solution 30 minutes.It is 3500 dialysis tubing good seal that irradiated mixing solutions is injected molecular weight cut-off; Dialysis tubing inserted in the de-ionized water-bath isolated unreacted vinylformic acid and ethanol in several hours; After from dialysis tubing, pour into solution in the beaker; And place 60 ℃ of baking oven numbers hour, obtain yellow or brown transparent colloidal liquid.Above-mentioned viscous fluid is dripped to dull and stereotyped going up continue drying, can obtain the organic polymer solid film of packaged silicon carbide nano particle.The solid film that generates is carried out the test of pl-collection of illustrative plates, and excitation wavelength is selected 300nm to 500nm, and every separated 20nm measures once, can obtain the photoluminescence spectrum of very strong luminous peak position with excitation wavelength adjustable (400 nm to 550 nm), and is as shown in Figure 2.
Claims (4)
1. method for preparing the polymer solids film that produces the tunable optical photoluminescence: it is characterized in that the suspension-s of 3C-SiC nano particle in water is added in vinylformic acid and the alcoholic acid mixing solutions priority carried out irradiation 1 ± 0.3 hour under blue light and 360 nm UV-lights; Superscribe one deck ROHM organic polymer at nano grain surface; Place dialysis tubing to clean out unreacted vinylformic acid and ethanol reacted solution; And place 60 ± 10 ℃ of baking ovens to concentrate several hours, obtain yellow or brown transparent colloidal liquid; Above-mentioned viscous fluid is dripped to dull and stereotyped going up continue drying, obtain the polymer solids film of packaged silicon carbide nano particle.
2. preparation according to claim 1 produces the method for the polymer solids film of tunable optical photoluminescence: it is characterized in that the 3C-SiC nano particle adopts the chemical corrosion method preparation: micron-sized 3C-SiC powder is positioned over beaker as etch reactants, and etching solution is 65 wt% nitric acid (HNO
3) and 40 wt% hydrofluoric acid (HF) composition, the volume ratio of nitric acid and hydrofluoric acid is 1:3, and the quality of etching solution is more than six times of 3C-SiC powder, and the etching reaction temperature is 100 ± 10 ° of C, and the reaction times is 1 ± 0.2 hour; After the reaction, the mixed liquid of gained acid and powder is cooled to room temperature, left standstill several hours or centrifugation after, skim the upper strata and react remaining acid solution, the powder that obtains is cleaned the back oven dry repeatedly with deionized water; Powder after the oven dry is positioned in the glass beaker, adds deionized water, about 30～60 minutes of sonic oscillation, with products therefrom left standstill several hours or centrifugation after, get supernatant liquid, get final product the suspension-s of 3C-SiC nano particle in water.
3. preparation according to claim 1 produces the method for the polymer solids film of tunable optical photoluminescence: it is characterized in that it is that 3500 dialysis tubing cleans out unreacted vinylformic acid and ethanol that reacted solution is placed molecular weight cut-off.
4. preparation as claimed in claim 1 produces the method for the polymer solids film of tunable optical photoluminescence, it is characterized in that the solid film that generates is that luminous peak position is with the adjustable photoluminescence spectrum of excitation wavelength 400 nm to 550 nm.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101058725A (en) * | 2007-06-05 | 2007-10-24 | 南京大学 | Method of preparing 3C-SiC nano particles by chemical corrosion method |
| CN102127432A (en) * | 2011-01-12 | 2011-07-20 | 南京大学 | 3C-SiC nanoparticle modifying method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101058725A (en) * | 2007-06-05 | 2007-10-24 | 南京大学 | Method of preparing 3C-SiC nano particles by chemical corrosion method |
| CN102127432A (en) * | 2011-01-12 | 2011-07-20 | 南京大学 | 3C-SiC nanoparticle modifying method |
Non-Patent Citations (3)
| Title |
|---|
| H.W.SHIM ET AL.: "Anomalous photoluminescence from 3C-SiC grown on Si(111) by rapid thermal chemical vapor deposition", 《APPL. PHYS. LETT.》, vol. 70, no. 13, 31 March 1997 (1997-03-31), pages 1757 - 1759 * |
| J. WANG ET AL.: "Glycerol-Bonded 3C-SiC Nanocrystal Solid Films Exhibiting Broad and Stable Violet to Blue-Green Emission", 《NANO LETT.》, vol. 10, 3 August 2010 (2010-08-03), pages 1466 - 1471 * |
| Z. F. LI ET AL.: "Water-Soluble Poly(acrylic acid) Grafted Luminescent Silicon Nanoparticles and Their Use as Fluorescent Biological Staining Labels", 《NANO LETTERS》, vol. 4, no. 8, 18 June 2004 (2004-06-18), pages 1463 - 1467 * |
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Application publication date: 20120815 |