CN101058725A - Method of preparing 3C-SiC nano particles by chemical corrosion method - Google Patents
Method of preparing 3C-SiC nano particles by chemical corrosion method Download PDFInfo
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- CN101058725A CN101058725A CN200710023478.6A CN200710023478A CN101058725A CN 101058725 A CN101058725 A CN 101058725A CN 200710023478 A CN200710023478 A CN 200710023478A CN 101058725 A CN101058725 A CN 101058725A
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- sic
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- deionized water
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- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000002105 nanoparticle Substances 0.000 title claims description 18
- 238000005260 corrosion Methods 0.000 title claims description 7
- 230000007797 corrosion Effects 0.000 title claims description 7
- 239000000126 substance Substances 0.000 title claims description 5
- 239000000843 powder Substances 0.000 claims abstract description 22
- 239000002253 acid Substances 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 4
- 239000006228 supernatant Substances 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 10
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000013049 sediment Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 13
- 239000002131 composite material Substances 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 238000005530 etching Methods 0.000 abstract 1
- 238000002604 ultrasonography Methods 0.000 abstract 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 32
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 15
- 239000000463 material Substances 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- -1 carbon ion Chemical class 0.000 description 3
- 230000005284 excitation Effects 0.000 description 3
- 238000000103 photoluminescence spectrum Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 229960004756 ethanol Drugs 0.000 description 2
- 229910001218 Gallium arsenide Inorganic materials 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
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000002950 deficient Effects 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
- 238000002474 experimental method Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 229910021426 porous silicon Inorganic materials 0.000 description 1
- 230000004223 radioprotective effect Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 230000004304 visual acuity Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a making method of 3C-SiC nanometer particle, which comprises the following steps: adopting the composite liquid of fluohydric acid, nitric acid to etch common 3C-SiC powder; using the size of original powder more than micrometer magnitude's; making the density of etching acid at 35%-45% and the density of nitric acid at 60%-70% with bulk rate at 2. 0-3. 0:1. 0; heating to 80-100 deg. c for 0. 5-2. 0h; cooling; blending reated acid liquid and powder in the high-speed centrifuger to centrifuge; pouring the upper-layer acid liquid; fetching the lower-layer powder; drying in the baker at 70-90 deg. c; adding centrifugal or anhydrous alcohol in the powder; cavitating through ultrasound for 30-60min; fetching the upper supernatant layer with 3C-SiC nanometer particle with size less than 8nm in the deionized water and anhydrous alcohol.
Description
Technical field
The present invention relates to a kind of simple, cheap, the 3C-SiC nanometer particle process method that can launch strong blue light, especially prepare particle diameter less than 8 nanometers, have the method for the 3C-SiC nano particle of strong blue emission performance.
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 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, andN.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)], 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 [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.
Summary of the invention
The objective of the invention is to overcome the defective of above-mentioned preparation 3C-SiC nano particle, propose a kind of simple, inexpensive method, especially prepare particle diameter less than 8 nanometers, have the method for the 3C-SiC nano particle of strong blue emission performance.
Technical scheme of the present invention is: chemical corrosion method prepares the method for 3C-SiC nano particle, with the common 3C-SiC powder of the mixed corrosion of hydrofluoric acid, nitric acid, described powder size is preferably micron dimension, this powder does not have obvious blue emission, it is the hydrofluoric acid of 35%-45% and the nitric acid of 60%-70% that general chemistry is corroded used acid concentration, and volume ratio is 2.0-3.0: 1.0.Mixing acid during reaction is more than 5-15 times of 3C-SiC powder, is heated to 80 ℃-100 ℃, and the reaction times is 0.5-2.0 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 70 ℃-90 ℃.In dried powder, add deionized water or dehydrated alcohol, ultrasonic cavitation 30-60 minute, leave standstill a few hours or centrifugation and remove the lower sediment thing, get 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 3C-SiC nano particle that in solution, can show strong blue emission, the size of nano particle is less than 8nm, average particle size particle size is about 3.8nm, the Bohr radius R of 3C-SiC is 2.7nm, obviously, the particulate mean radius is less than R, so can cause showing that well quantum limitation effect will appear in its photoluminescence spectrum in the solution or film of passivation.When excitation wavelength when 320nm increases to 440nm, radiative glow peak will be increased to 480nm from 430nm.
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 is the transmission electron microscope photo that the present invention is prepared in the 3C-SiC nano particle in the ethanol.(a) and enlargement ratio (b) be respectively 15000 times with 97000 times.
Fig. 2 be the present invention be prepared in ethanol (Fig. 2 a) with deionized water (Fig. 2 b) in the photoluminescence spectrum of 3C-SiC nano particle, excitation wavelength is 300nm, 340nm, 380nm and 420nm.
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.
The size of high resolving power electron photomicrograph explanation nano particle is less than 8.0nm.Photoluminescence spectrum show when excitation wavelength when 320nm increases to 440nm, radiative glow peak is increased to 480nm from 430nm.
Claims (1)
1, chemical corrosion method prepares the method for 3C-SiC nano particle, it is characterized in that the common 3C-SiC powder of mixed corrosion with hydrofluoric acid, nitric acid, used starting powder yardstick is greater than micron dimension, corrode hydrofluoric acid that used acid is concentration 35%-45% and the nitric acid of concentration 60%-70%, volume ratio is 2.0-3.0: 1.0; Mixing acid during reaction is more than 5-15 times of 3C-SiC powder, is heated to 80 ℃-100 ℃, and the reaction times is 0.5-2.0 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, 70 ℃-90 ℃ are carried out drying in baking oven; In dried powder, add deionized water or dehydrated alcohol, ultrasonic cavitation 30-60 minute, leave standstill a few hours or centrifugation and remove the lower sediment thing, get supernatant liquid; Promptly contain the 3C-SiC nano particle of size in this deionized water or the dehydrated alcohol clear liquid less than 8nm.
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|---|---|---|---|
| CNB2007100234786A CN100551997C (en) | 2007-06-05 | 2007-06-05 | Chemical corrosion method prepares the method for 3C-SiC nano particle |
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| CNB2007100234786A CN100551997C (en) | 2007-06-05 | 2007-06-05 | Chemical corrosion method prepares the method for 3C-SiC nano particle |
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| CN101058725A true CN101058725A (en) | 2007-10-24 |
| CN100551997C CN100551997C (en) | 2009-10-21 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102127432A (en) * | 2011-01-12 | 2011-07-20 | 南京大学 | 3C-SiC nanoparticle modifying method |
| CN102590154A (en) * | 2012-01-11 | 2012-07-18 | 南京大学 | Method for measuring intracellular pH value by using 3C-SiC nano-particle photoluminescence spectrum |
| CN102634338A (en) * | 2012-04-09 | 2012-08-15 | 南京大学 | Preparing method of tunable photoluminescence polymer solid thin film |
| CN103441063A (en) * | 2013-05-31 | 2013-12-11 | 西安交通大学 | Method for preparing silicon carbide micro-structures |
-
2007
- 2007-06-05 CN CNB2007100234786A patent/CN100551997C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102127432A (en) * | 2011-01-12 | 2011-07-20 | 南京大学 | 3C-SiC nanoparticle modifying method |
| CN102590154A (en) * | 2012-01-11 | 2012-07-18 | 南京大学 | Method for measuring intracellular pH value by using 3C-SiC nano-particle photoluminescence spectrum |
| CN102634338A (en) * | 2012-04-09 | 2012-08-15 | 南京大学 | Preparing method of tunable photoluminescence polymer solid thin film |
| CN103441063A (en) * | 2013-05-31 | 2013-12-11 | 西安交通大学 | Method for preparing silicon carbide micro-structures |
| CN103441063B (en) * | 2013-05-31 | 2016-06-08 | 西安交通大学 | A kind of preparation method of carborundum micro structure |
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| Publication number | Publication date |
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| CN100551997C (en) | 2009-10-21 |
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Granted publication date: 20091021 Termination date: 20110605 |