CN102127432A - 3C-SiC nanoparticle modifying method - Google Patents
3C-SiC nanoparticle modifying method Download PDFInfo
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- CN102127432A CN102127432A CN2011100055890A CN201110005589A CN102127432A CN 102127432 A CN102127432 A CN 102127432A CN 2011100055890 A CN2011100055890 A CN 2011100055890A CN 201110005589 A CN201110005589 A CN 201110005589A CN 102127432 A CN102127432 A CN 102127432A
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- 239000002105 nanoparticle Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 21
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 57
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 230000010355 oscillation Effects 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 9
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 6
- 230000004048 modification Effects 0.000 claims description 6
- 238000012986 modification Methods 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 229960004756 ethanol Drugs 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 abstract description 40
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 abstract description 18
- 239000000463 material Substances 0.000 abstract description 9
- 238000002474 experimental method Methods 0.000 abstract description 4
- KXCPAUWIRBMTET-SOFGYWHQSA-N (6e)-8-methyl-5-propan-2-ylnona-6,8-dien-2-ol Chemical compound CC(O)CCC(C(C)C)\C=C\C(C)=C KXCPAUWIRBMTET-SOFGYWHQSA-N 0.000 abstract 1
- 239000008279 sol Substances 0.000 description 15
- 239000002245 particle Substances 0.000 description 11
- 238000002161 passivation Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 229910021426 porous silicon Inorganic materials 0.000 description 5
- 238000000103 photoluminescence spectrum Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- -1 carbon ion Chemical class 0.000 description 3
- 230000005284 excitation Effects 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 229910008051 Si-OH Inorganic materials 0.000 description 1
- 229910006358 Si—OH Inorganic materials 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 229940053080 isosol Drugs 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 230000004223 radioprotective effect Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000004304 visual acuity Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
The invention relates to a simple and cheap 3C-SiC nanoparticle modifying method, which comprises: adding glycerol into 3C-SiC nanoparticle sol; and mixing and performing ultrasonic oscillation to disperse 3C-SiC nanoparticles. The preferred ultrasonic oscillation time is 30 to 60 minutes. Preferably, at least 0.2ml of glycerol is added into each 10ml of sol. The sol is aqueous sol or ethanol sol. The invention has the advantages that: the preparation method is simple; complex experiment devices are not required; the experiment material is cheap and can be obtained easily; and the prepared silicon carbide nanoaparticles emit strong and stable blue light.
Description
Technical field
The present invention relates to a kind of simply, cheap, can improve the luminous method of 3C-SiC nanoparticle, improve luminous intensity, the method for stability and controllability.
Background technology
Silicon carbide is the third generation wide bandgap semiconductor materials that grows up after first elemental semiconductors (Si) and s-generation compound semiconductor materials GaAs, GaP and the InP.Silicon carbide not only has bigger band gap width (3C, 4H, 6H type silicon carbide band gap width at room temperature are respectively 2.24,3.22,2.86eV), 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 silicon carbide, 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 has bigger band gap width (2.24eV), its light-emitting zone still in the scope of green glow, and because silicon carbide is a kind of indirect band-gap semiconductor material, at room temperature luminous very faint of the carbofrax material of body material.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 silicon carbide 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, silicon carbide has goodish bio-compatibility, particularly with the compatibility of blood, and the density of SiC is less, chemical stability 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.
Nanometer silicon carbide particulate preparation in the past is main to be realized by two kinds of methods.First method is to generate the nanometer silicon carbide particle by various chemical reactions, injects silicon chip [L.S.Liao, X.M.Bao such as carbon ion, Z.F.Yang, and N.B.Min, Appl.Phys.Lett.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)], C60 coupling porous silicon [X.L.Wu, G.G.Siu, M.J.Stokes, D.L.Fan, Y.Gu, and X.M.Bao, preparation method but these methods all can not prepare the single structure phase such as Appl.Phys.Lett.77,1292 (2000)], the nano particle of 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 [X.L.Wu of emissive porwer, J.Y.Fan, T.Qiu, X.Yang, G.G.Siu, and P.K.Chu, Phys.Rev.Lett.94,026102 (2005)], but this method preparation process relative complex be 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
The objective of the invention is to overcome the defective of above-mentioned 3C-SiC nano particle, propose a kind of method of modifying of simple, cheap 3C-SiC nano particle.
Technical scheme of the present invention is: the method for modifying of 3C-SiC nano particle, glycerol is added the colloidal sol of 3C-SiC nano particle, and carry out sonic oscillation after the mixing, make the 3C-SiC nanoparticulate dispersed.
The sonic oscillation time is 30-60min.
Every 100ml colloidal sol is put into the 0.2ml glycerol at least.Glycerol is that passivation effect is bad very little, and glycerol is too many, and to the not influence of particulate luminosity, but because glycerol is difficult for evaporation, the colloidal sol after the modification has the residual of glycerol when making film, so the consumption of glycerol is preferably 0.2-0.4ml.
Described colloidal sol is the water-sol or ethanol colloidal sol.The preparation method of described colloidal sol is a prior art: 3C-SiC powder 10g is added among the mixed sour 100-110ml, reacting by heating (generally at 100-110 ℃ of heating 1h), after the cooling that reacted acid solution is centrifugal with powder, fall to remove the upper strata acid solution, take off a layer powder, dry, in dried powder, add deionized water or dehydrated alcohol 50-60ml, ultrasonic cavitation, leave standstill or centrifugal, get supernatant liquid, described mixing acid is that 3: 1～3.5: 1 40% hydrofluoric acid and 65% nitric acid are formed by volume ratio.
The 3C-SiC nano particle that in solution, can show strong blue emission, the size of used nano particle is less than 8nm, average particle size particle size is about 3.8nm, constant through particle size after the glycerol passivation, the surface is by well passivation modification, by XPS spectrum Si-OH is arranged as can be seen, this explanation nanometer silicon carbide particle surface is hung with the glycerol molecule, the energy density that is drawn by Theoretical Calculation and the original as can be seen discrete energy levels of PL collection of illustrative plates of experiment measuring gained become continuous energy level, the Bohr radius R of 3C-SiC is 2.7nm, obviously, the particulate mean radius is less than R, by glycerol after the good passivation excessively, quantum limitation effect will appear in its photoluminescence spectrum on the surface.When excitation wavelength when 320nm increases to 440nm, radiative glow peak will be increased to 480nm from 430nm.In air ambient, place after 6 months luminous still very stable, without any decay.
The invention has the advantages that the preparation method is simple, need not complicated experimental installation, the cheap and more easily acquisition of experiment material, the nanometer silicon carbide particulate blue emission of preparation is strong and stable.Other advantages of the present invention and effect will continue to describe below.
Description of drawings
Fig. 1---be prepared in the transmission electron microscope photo of the 3C-SiC nano particle in the ethanol.(a) and enlargement ratio (b) be respectively 15000 times with 97000 times.
Fig. 2---the photoluminescence spectrum of the 3C-SiC colloidal sol after the glycerol passivation, excitation wavelength by 320 to 460nm.
Fig. 3---the XPS of the 3C-SiC colloidal sol after the glycerol passivation.
The energy state density of Fig. 4---Theoretical Calculation gained, a, b, c are respectively each nano particle and hang 0,2,5 glycerol molecule.
Fig. 5---attached to the PL spectrum of the sol pellicle on the porous silicon.
Embodiment
It is 40% hydrofluoric acid and 65% nitric acid that general chemistry is corroded used acid, and volume ratio is 3: 1.Take by weighing 3C-SiC powder 10g during preparation, add among the above mixed sour 100ml, 100 ℃ of heating of thermostatic bath 1 hour.After the cooling that reacted acid solution is centrifugal in supercentrifuge with powder, fall to remove the upper strata acid solution, take off a layer powder, in baking oven, carry out drying about 80 ℃.Add deionized water or dehydrated alcohol in dried powder, ultrasonic cavitation 30 minutes leaves standstill a few hours or centrifugal, gets supernatant liquid.Promptly contain the 3C-SiC nano particle of size in this deionized water or the dehydrated alcohol clear liquid less than 8nm.The mean sizes of this nanoparticle is about 3.8nm.
Get the 100ml water-sol, add about 0.2ml glycerol, mix back sonic oscillation 30min, obtain the 3C-SiC nano particle colloidal sol after the modification.Porous silicon chip is put into the beaker that capacity is 10ml, in beaker, fill the colloidal sol of the modified carbonize silicon sol for preparing then, beaker is put into the ultrasonic evaporation of ultrasonic apparatus, porous silicon surface has just adhered to the nanometer silicon carbide particle film after one deck modification behind the whole evaporates to dryness of isosol again.
The size constancy of nano particle all less than 8.0nm, because the glycerol molecule is too little, can't arrive by electron microscopic observation before and after the high resolving power electron photomicrograph explanation modification.Photoluminescence spectrum show when excitation wavelength when 320nm increases to 460nm, radiative glow peak is increased to 530nm from 380nm, light emitting region became 360nm-760nm after this colloidal sol made film attached to the porous silicon substrate, had realized the photoluminescence of all wave band controllable light.In air ambient, place after 6 months luminous still very stable, without any decay.
Claims (6)
1. the method for modifying of a 3C-SiC nano particle is characterized in that glycerol is added the colloidal sol of 3C-SiC nano particle carrying out sonic oscillation after the mixing, makes the 3C-SiC nanoparticulate dispersed.
2. the method for modifying of 3C-SiC nano particle as claimed in claim 1 is characterized in that the sonic oscillation time is 30-60min.
3. the method for modifying of 3C-SiC nano particle as claimed in claim 1 is characterized in that every 100ml colloidal sol puts into the 0.2ml glycerol at least.
4. as the method for modifying of each described 3C-SiC nano particle among the claim 1-3, it is characterized in that described colloidal sol is the water-sol or ethanol colloidal sol.
5. the method for modifying of 3C-SiC nano particle as claimed in claim 4, the preparation method who it is characterized in that described colloidal sol is: 3C-SiC powder 10g is added among the mixed sour 100-110ml, reacting by heating, after the cooling that reacted acid solution is centrifugal with powder, fall to remove the upper strata acid solution, take off a layer powder, dry, in dried powder, add deionized water or dehydrated alcohol 50-60ml, ultrasonic cavitation, leave standstill or centrifugal, get supernatant liquid, described mixing acid is that 3: 1～3.5: 1 40% hydrofluoric acid and 65% nitric acid are formed by volume ratio.
6. as the method for modifying of each described 3C-SiC nano particle among the claim 1-3, it is characterized in that modification before, the 3C-SiC nanoparticle size in the colloidal sol is less than 8nm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102634338A (en) * | 2012-04-09 | 2012-08-15 | 南京大学 | Preparing method of tunable photoluminescence polymer solid thin film |
| CN102766459A (en) * | 2012-07-12 | 2012-11-07 | 复旦大学 | Post-treatment method of fluorescent powder for lamp |
| CN104593746A (en) * | 2014-10-29 | 2015-05-06 | 北京工业大学 | 3C-SiC nanometer disc and preparation method thereof |
Citations (1)
| 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 |
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Patent Citations (1)
| 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 |
Non-Patent Citations (2)
| Title |
|---|
| J.WANG,ET AL.: "Glycerol-Bonder 3C-SiC Nanocrystal Solid Films Exhibiting Broad and Stable Violet to Blue-Green Emission", 《NANO LETTERS》, vol. 10, 8 March 2010 (2010-03-08), pages 1466 - 1471 * |
| X.L.WU,ET AL.: "Identification of Surface Structures on 3C-SiC Nanocrystals with Hydrogen and Hydroxyl bonding by Photoluminescence", 《NANO LETTERS》, vol. 9, 6 November 2009 (2009-11-06), pages 4053 - 4060 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102634338A (en) * | 2012-04-09 | 2012-08-15 | 南京大学 | Preparing method of tunable photoluminescence polymer solid thin film |
| CN102766459A (en) * | 2012-07-12 | 2012-11-07 | 复旦大学 | Post-treatment method of fluorescent powder for lamp |
| CN104593746A (en) * | 2014-10-29 | 2015-05-06 | 北京工业大学 | 3C-SiC nanometer disc and preparation method thereof |
| CN104593746B (en) * | 2014-10-29 | 2017-07-14 | 北京工业大学 | One kind prepares 3C SiC nanometer plates, preparation method |
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Application publication date: 20110720 |