CN102268253A - Preparation method of low-cost cadmium phosphide quantum dot material - Google Patents
Preparation method of low-cost cadmium phosphide quantum dot material Download PDFInfo
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- CN102268253A CN102268253A CN2011101562888A CN201110156288A CN102268253A CN 102268253 A CN102268253 A CN 102268253A CN 2011101562888 A CN2011101562888 A CN 2011101562888A CN 201110156288 A CN201110156288 A CN 201110156288A CN 102268253 A CN102268253 A CN 102268253A
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Abstract
The invention discloses a preparation method of a low-cost cadmium phosphide quantum dot material. The preparation method comprises the following steps: based on a cheap cadmium compound such as cadmium oxide, cadmium acetate or cadmium cetylacetonate and the like as a raw material, dissolving the cadmium compound and long-chain fatty acid in octadecylene at a high temperature so as to prepare a long-chain fatty acid salt of cadmium; or dissolving cadmium cetylacetonate in organic amine, and then carrying out a gas-liquid reaction based on hydrogen phosphide as a phosphorus source so as to prepare the high-quality cadmium phosphide quantum dot luminescent material. According to the invention, a cheap and continuously operable synthesis method is provided for the cadmium phosphide quantum dot material, and a solid foundation is provided for industrialized production of the cadmium phosphide quantum dot material; and through controlling factors such as reaction temperature, time and the like, the luminescence of the cadmium phosphide quantum dot material can be achieved in a wide region ranging from visible light (460nm) to infrared light (1500nm).
Description
One, technical field
The present invention relates to a kind of preparation of nanomaterials, specifically a kind of preparation method of low-cost cadmium phosphide quanta point material.
Two, background technology
Cadmium phosphide is a kind of important II-V family semiconductor material, because cadmium phosphide has narrower bandwidth (0.55eV), higher dielectric constant (5.8), very big Bohr radius (18nm) and exciton have very light advantages such as virtual mass [1-4], be expected at biomarker, fluorescent probe, opto-electronic conversion is applied in the fields such as solar cell [5-8].When semi-conductive size during less than Bohr radius, its quantum size effect performance obviously, size reduces, the absorption spectrum peak shows as blue shift.Because cadmium phosphide has smaller energy gap [3], therefore, along with reducing of its physical size, can realize large-scale conciliation from infrared to the visible region, this character can make cadmium phosphide at biological fluorescent labelling, and numerous areas such as photoelectric commutator and solar cell material have wide practical use.
But by the end of at present, the synthetic method that relates to cadmium phosphide quanta point material or cadmium phosphide nanocrystal is still with organometallics (Cd[P (SiPh
3)]
2, [MeCdPBu
2]
3, Me
2Cd and HPBu
2Ph=phenyl, Bu=butyl, Me=methyl) thermolysis, methods such as alcoholysis prepare, and perhaps adopt with 3-3, methyl-silylation phosphide is the synthetic cadmium phosphide quantum dot [9-14] of the hot injection in phosphorus source.Their common weakness are exactly that presoma is very expensive, and transportation, storage condition harshness, and compound experiment is difficult to be exaggerated, thereby does not have industrialization prospect.Along with the optical property of cadmium phosphide, the research of photoelectrochemistry character and photoelectric device becomes better and approaching perfection day by day, and the cadmium phosphide synthesis technique of Sheng Chaning becomes the focus of people's attention low-costly and in high volume.
Reference:
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[2]Schaller，R.D.；Klimov，V.I.Phys.Rev.Lett.2004，92(18)，186601-1.
[3]V.I.Klimov，A.A.Mikhailovsky，S.Xu，J.A.Holligsworth，C.A.Leatherdale，H.J.Eisler?and?M.G.Bawendi，Science，2000，290，314.
[4]Schlamp，M.C.；Peng，X.；Alivisatos，A.P.J.Appl.Phys.1997，82，5837-5842.
[5]Mattoussi，H.；Radzilowski，L.H.；Dabbousi，B.O.；Thomas，E.L.；Bawendi，M.G.；Rubner，M.F.J.Appl.Phys.1998，83，7965-7974.
[6]Goel，S.C.；Chang，M.Y.；E.Buhro，W.J.Am.Chem.Soc.1990，112，5636.
[7]Matchett，M.A.；Viano，A.M.;Adolphi，N.L.；Stoddard，R.D.；Buhro，W.E.；Conradi，M.S.；Gibson，P.C.Chem.Mater.1992，4，508.
[8]B.L.Benac，A.H.Cowly，R.A.Jones，C.M.Nunn，T.C.Wright，J.Am.Chem.Soc.1989，111，4986.
[9]Green，M.；O′Brien，P.Adv.Mater.1998，10，527.
[10]Nigel?Pickett，US?2007/0104865?A1.
[11]Green，M.；O′Brien，P.J.Mater.Chem.1999，9，243.
[12]Wang，R.；Ratcliffe，C.I.；Wu，X.；Voznyy，O.；Tao，Y.；Yu，K.J.Phys.Chem.C?2009，113，17979.
[13]S.D.Miao，S.G.Hickey，B.Rellinghaus，C.Waurisch，A.Eychmüller，J.Am.Chem.Soc.，2010，132(16)，5613-5615.
[14]R.G.Xie，J.X.Zhang，F.Zhao，W.S.Yang，X.G.Peng，Chem.Mater.，2010，22(13)，3820-3822.
Three, summary of the invention
The present invention is for fear of above-mentioned existing in prior technology weak point, aims to provide that a kind of preparation method is simple, with low cost, the preparation method of the low-cost cadmium phosphide quanta point material that is easy to industrialization.
The present invention is a solvent with nonpolar, high boiling octadecylene or organic amine, and the presoma with cadmium is dissolved in wherein under certain condition, forms the hard soap octadecylene solution of cadmium or the organic amine solution of methyl ethyl diketone cadmium, feeds PH under the certain temperature condition
3Gas makes the cadmium phosphide quanta point material.
Technical solution problem of the present invention adopts following technical scheme:
The preparation method's of the low-cost cadmium phosphide quanta point material of the present invention characteristics are to operate according to the following steps:
The preparation of a, cadmium presoma
Cadmic compound and 4mmol with 2mmol, longer chain fatty acid join in the there-necked flask that contains the 15mL octadecylene, cadmium ion and hydrionic mol ratio are 1: 2, in nitrogen atmosphere in 260-280 ℃ of insulation reaction 20 minutes, obtain the soap solution of water white cadmium, i.e. the cadmium precursor solution; Or the methyl ethyl diketone cadmium of 2mmol is dissolved in the 10-20mL organic amine, at N
2Be heated to 80-150 ℃ in the atmosphere, obtain the organic amine solution of orange-yellow methyl ethyl diketone cadmium, i.e. the cadmium precursor solution;
The preparation of b, cadmium phosphide quantum dot
The temperature of the soap solution of the cadmium that step a is obtained is controlled at 60-320 ℃, and is down auxiliary in stream of nitrogen gas, feeds PH
3Gas, N
2With PH
3Velocity ratio be 1-15: 1, insulation reaction 2-180min obtains the octadecylene solution of cadmium phosphide quantum dot; The temperature of the organic amine solution of the methyl ethyl diketone cadmium that step a is obtained is controlled at 80-200 ℃, and is down auxiliary in stream of nitrogen gas, feeds PH
3Gas, N
2With PH
3Velocity ratio be 1-15: 1, insulation reaction 2-180min obtains the organic amine solution of cadmium phosphide quantum dot;
Described PH
3Can be by prices such as calcium phosphide or zinc phosphide cheap compound and H
2SO
4Synthetic obtaining also can directly be bought PH
3Gas; Calcium phosphide and zinc phosphide are cheap, and be stable in the air, easily transportation and preservation.
C, separation are purified
In the organic amine solution of the octadecylene solution of the cadmium phosphide quantum dot that step b obtains or cadmium phosphide quantum dot, add 20mL toluene, extracting and separating is left and taken upper solution, in described upper solution, add 20mL Virahol and 10mL methyl alcohol, solid phase is reclaimed in centrifugation, and re-extract, centrifugal process promptly get the cadmium phosphide quanta point material 3-5 time.The cadmium phosphide quanta point material can be dissolved in the non-polar solvent again, as toluene, and n-hexane, chloroform etc.
The preparation method's of the low-cost cadmium phosphide quanta point material of the present invention characteristics also are: described cadmic compound is Cadmium oxide, cadmium acetate or methyl ethyl diketone cadmium.
The preparation method's of the low-cost cadmium phosphide quanta point material of the present invention characteristics also are: described longer chain fatty acid is meant that carbon atom number is not less than 12 saturated or unsaturated fatty acids in the main chain.
The preparation method's of the low-cost cadmium phosphide quanta point material of the present invention characteristics also are: described longer chain fatty acid is lauric acid, myristic acid, palmitinic acid, physetoleic acid, oleic acid, stearic acid, Palmiticacid, eicosanoic acid, mountain Yu acid or cerinic acid.
The preparation method's of the low-cost cadmium phosphide quanta point material of the present invention characteristics also are: described organic amine is meant that carbon atom number is not less than 6 saturated or unsaturated fatty acids amine in the main chain.
The preparation method's of the low-cost cadmium phosphide quanta point material of the present invention characteristics also are: described organic amine is an oleyl amine.
The formation reaction of described cadmium phosphide quantum dot all be under solution condition with PH
3Gas reaction has different solvent temperatures for different lipid acid, so temperature of reaction will adjust with the chain length of soap, generally all about 60-320 ℃.
The photoluminescence effect:
The cadmium phosphide that obtains is dissolved in toluene or the zellon, gets the quartz cell that the 2mL sample places 1 centimetre,, obtain the abosrption spectrogram of cadmium phosphide by investigating absorption spectrum from 2000nm to the 300nm wavelength region; Adopt the 400nm exciting light, by fluorescence spectrophotometer, measure the fluorescence spectrum of cadmium phosphide, wherein as seen toluene be suitable for-mensuration of ultraviolet band as solvent, the mensuration of zellon is suitable for infrared-visible waveband.(median size 1.8～12nm) can realize the emission wavelength scope of 460～1500nm to size by control cadmium phosphide quantum dot.
Compared with the prior art, beneficial effect of the present invention is embodied in:
1, the presoma of cadmium used in the present invention and phosphorus is the stable compound of physicochemical property in the air, and synthetic method is simple, but operate continuously, and test dose amplifies easily, is a green technology.
2, the present invention compared production cost and is reduced to original 19% with former synthetic method.
3, cadmium phosphide product yield of the present invention reaches 97%.
4, the inventive method realizes separating of product and solvent easily, and high boiling lipid acid can be recycled.
5, by regulating synthesis temperature and reaction times, synthetic product of the present invention can be realized luminous from 460nm to the 1500nm wave band, and the quantum yield of its photoluminescence reaches more than 25%.
Four, description of drawings
Fig. 1 is the in kind photo of cadmium phosphide under ultra violet lamp that the present invention prepares.
Fig. 2 a and Fig. 2 b are the UV-Vis-IR abosrption spectrograms of the cadmium phosphide quantum dot solution for preparing of the present invention, and wherein Fig. 2 b is that Fig. 2 a is at the spectrum enlarged view of absorbancy less than 0.09 zone.
Fig. 3 is photoluminescence (fluorescence spectrum) spectrogram of the cadmium phosphide for preparing of the present invention.
Fig. 4 is the projection electron microscope figure of the cadmium phosphide (luminous maximum wavelength is 1250nm) for preparing of the present invention.
Five, embodiment
The PH that uses among the embodiment 1-11
3For by calcium phosphide or zinc phosphide and H
2SO
4Reaction obtains or is commercial obtaining according to a conventional method; Calcium phosphide and zinc phosphide are cheap, and be stable in the air, easily transportation and preservation.
Embodiment 1:
The preparation method of low-cost cadmium phosphide quanta point material operates according to the following steps in the present embodiment:
The preparation of a, cadmium presoma
Cadmium oxide 0.258g and 1.3mL oleic acid are placed the 25mL there-necked flask, add the 15mL octadecylene, room temperature vacuumized (0.5-0.05mbar) 30 minutes, was heated to 270 ℃ then in nitrogen atmosphere, and insulation reaction obtained cadmium oleate solution in 20 minutes;
The preparation of b, cadmium phosphide quantum dot
The temperature of gained cadmium oleate solution is controlled at 60 ℃, down auxiliary in stream of nitrogen gas, feed PH
3Gas, PH
3Flow velocity is 2mL/min, carrier gas N
2Flow velocity is 30mL/min, N
2With PH
3Velocity ratio be 15: 1, insulation reaction 180min obtains the octadecylene solution of cadmium phosphide quantum dot, yield 97.5%;
C, separation are purified
In the octadecylene solution of cadmium phosphide quantum dot, add 20mL toluene, extracting and separating is left and taken upper solution, add 20mL Virahol and 10mL methyl alcohol in upper solution, solid phase is reclaimed in centrifugation, and re-extract, centrifugal process promptly get the cadmium phosphide quanta point material 3-5 time.
Embodiment 2:
The preparation method of low-cost cadmium phosphide quanta point material operates according to the following steps in the present embodiment:
The preparation of a, cadmium presoma
Cadmium oxide 0.258g and 0.8g lauric acid are placed the 25mL there-necked flask, add the 15mL octadecylene, room temperature vacuumized (0.5-0.05mbar) 30 minutes, was heated to 250 ℃ then in nitrogen atmosphere, and insulation reaction obtained cadmium laurate solution in 20 minutes;
The preparation of b, cadmium phosphide quantum dot
The temperature of gained cadmium laurate solution is controlled at 120 ℃, down auxiliary in stream of nitrogen gas, feed PH
3Gas, PH
3Flow velocity is 2mL/min, carrier gas N
2Flow velocity is 2mL/min, N
2With PH
3Velocity ratio be 1: 1, insulation reaction 120min obtains the octadecylene solution of cadmium phosphide quantum dot, yield 97.0%;
The method that c, separation are purified is with embodiment 1.
Embodiment 3:
The preparation method of low-cost cadmium phosphide quanta point material operates according to the following steps in the present embodiment:
The preparation of a, cadmium presoma
Cadmium oxide 0.258g and 1.05g palmitinic acid are placed the 25mL there-necked flask, add the 15mL octadecylene, room temperature vacuumized (0.5-0.05mbar) 30 minutes, was heated to 260 ℃ then in nitrogen atmosphere, and insulation reaction obtained the palmitinic acid cadmium solution in 20 minutes;
The preparation of b, cadmium phosphide quantum dot
The temperature of gained palmitinic acid cadmium solution is controlled at 180 ℃, down auxiliary in stream of nitrogen gas, feed PH
3Gas, PH
3Flow velocity is 2mL/min, carrier gas N
2Flow velocity is 20mL/min, N
2With PH
3Velocity ratio be 10: 1, insulation reaction 30min obtains the octadecylene solution of cadmium phosphide quantum dot, yield 97.3%;
The method that c, separation are purified is with embodiment 1.
Embodiment 4:
The preparation method of low-cost cadmium phosphide quanta point material operates according to the following steps in the present embodiment:
The preparation of a, cadmium presoma
Cadmium oxide 0.258g and 1.0g myristic acid are placed the 25mL there-necked flask, add the 15mL octadecylene, room temperature vacuumized (0.5-0.05mbar) 30 minutes, was heated to 260 ℃ then in nitrogen atmosphere, and insulation reaction obtained the myristic acid cadmium solution in 20 minutes;
The preparation of b, cadmium phosphide quantum dot
The temperature of gained myristic acid cadmium solution is controlled at 220 ℃, down auxiliary in stream of nitrogen gas, feed PH
3Gas, PH
3Flow velocity is 2mL/min, carrier gas N
2Flow velocity is 4mL/min, N
2With PH
3Velocity ratio be 2: 1, insulation reaction 20min obtains the octadecylene solution of cadmium phosphide quantum dot, yield 98.1%;
The method that c, separation are purified is with embodiment 1.
Embodiment 5:
The preparation method of low-cost cadmium phosphide quanta point material operates according to the following steps in the present embodiment:
The preparation of a, cadmium presoma
Cadmium oxide 0.258g and 1.14g stearic acid are placed the 25mL there-necked flask, add the 15mL octadecylene, 100 ℃ of following vacuum are extracted volatilizable solvent out, are heated to 250 ℃ then in nitrogen atmosphere, and insulation reaction obtained cadmium stearate solution in 20 minutes;
The preparation of b, cadmium phosphide quantum dot
The temperature of gained cadmium stearate solution is controlled at 320 ℃, down auxiliary in stream of nitrogen gas, feed PH
3Gas, PH
3Flow velocity is 2mL/min, carrier gas N
2Flow velocity is 10mL/min, N
2With PH
3Velocity ratio be 5: 1, insulation reaction 2min obtains the octadecylene solution of cadmium phosphide quantum dot, yield 96.5%;
The method that c, separation are purified is with embodiment 1.
Embodiment 6:
The preparation method of low-cost cadmium phosphide quanta point material operates according to the following steps in the present embodiment:
The preparation of a, cadmium presoma
Cadmium oxide 0.258g and 1.8g eicosanoic acid are placed the 25mL there-necked flask, add the 15mL octadecylene, room temperature vacuumized (0.5-0.05mbar) 30 minutes, was heated to 270 ℃ then in nitrogen atmosphere, and insulation reaction obtained the eicosanoic acid cadmium solution in 20 minutes;
The preparation of b, cadmium phosphide quantum dot
The temperature of gained eicosanoic acid cadmium solution is controlled at 250 ℃, down auxiliary in stream of nitrogen gas, feed PH
3Gas, PH
3Flow velocity is 2mL/min, carrier gas N
2Flow velocity is 20mL/min, N
2With PH
3Velocity ratio 10: 1, be insulation reaction 10min, obtain the octadecylene solution of cadmium phosphide quantum dot, yield 94.3%;
The method that c, separation are purified is with embodiment 1.
Embodiment 7:
The preparation method of low-cost cadmium phosphide quanta point material operates according to the following steps in the present embodiment:
The preparation of a, cadmium presoma
Cadmium oxide 0.258g and the Yu acid of 2.0g mountain are placed the 25mL there-necked flask, add the 15mL octadecylene, room temperature vacuumized (0.5-0.05mbar) 30 minutes, was heated to 270 ℃ then in nitrogen atmosphere, and insulation reaction obtained mountain Yu acid cadmium solution in 20 minutes;
The preparation of b, cadmium phosphide quantum dot
The temperature of gained mountain Yu acid cadmium solution is controlled at 250 ℃, down auxiliary in stream of nitrogen gas, feed PH
3Gas, PH
3Flow velocity is 2mL/min, carrier gas N
2Flow velocity is 30mL/min, N
2With PH
3Velocity ratio be 15: 1, insulation reaction 10min obtains the octadecylene solution of cadmium phosphide quantum dot, yield 96.8%;
The method that c, separation are purified is with embodiment 1.
Embodiment 8:
The preparation method of low-cost cadmium phosphide quanta point material operates according to the following steps in the present embodiment:
The preparation of a, cadmium presoma
Cadmium oxide 0.258g and 1.25mL linolic acid are placed the 25mL there-necked flask, add the 15mL octadecylene, room temperature vacuumized (0.5-0.05mbar) 30 minutes, was heated to 270 ℃ then in nitrogen atmosphere, and insulation reaction obtained the linolic acid cadmium solution in 20 minutes;
The preparation of b, cadmium phosphide quantum dot
The temperature of gained linolic acid cadmium solution is controlled at 250 ℃, down auxiliary in stream of nitrogen gas, feed PH
3Gas, PH
3Flow velocity is 2mL/min, carrier gas N
2Flow velocity is 4mL/min, N
2With PH
3Velocity ratio be 2: 1, insulation reaction 10min obtains the octadecylene solution of cadmium phosphide quantum dot, yield 98.5%;
The method that c, separation are purified is with embodiment 1.
Embodiment 9:
The preparation method of low-cost cadmium phosphide quanta point material operates according to the following steps in the present embodiment:
The preparation of a, cadmium presoma
Cadmium diacetate dihydrate 0.53g and 1.3mL oleic acid are placed the 25mL there-necked flask, add the 15mL octadecylene, extract volatilizable solvent under 100 ℃ of conditions out, be heated to 250 ℃ then in nitrogen atmosphere, insulation reaction obtained cadmium oleate solution in 20 minutes;
The preparation of b, cadmium phosphide quantum dot
The temperature of gained cadmium oleate solution is controlled at 280 ℃, down auxiliary in stream of nitrogen gas, feed PH
3Gas, PH
3Flow velocity is 2mL/min, carrier gas N
2Flow velocity is 20mL/min, N
2With PH
3Velocity ratio be 10: 1, insulation reaction 5min obtains the octadecylene solution of cadmium phosphide quantum dot, yield 90.5%;
The method that c, separation are purified is with embodiment 1.
Embodiment 10:
The preparation of a, cadmium presoma
Methyl ethyl diketone cadmium 0.62g and 15mL oleyl amine are placed the 25mL there-necked flask, extract volatilizable solvent under 100 ℃ of conditions out, at N
2Insulation reaction 20min obtains cadmium oleate solution in the atmosphere;
The preparation of b, cadmium phosphide quantum dot
The temperature of cadmium oleate solution is controlled at 80 ℃, down auxiliary in stream of nitrogen gas, feed PH
3Gas, PH
3Flow velocity is 2mL/min, carrier gas N
2Flow velocity is 20mL/min, N
2With PH
3Velocity ratio be 10: 1, insulation reaction 180min obtains the oleyl amine solution of cadmium phosphide quantum dot, yield 94.8%;
C, separation are purified
In the oleyl amine solution of cadmium phosphide quantum dot, add 20mL toluene, extracting and separating is left and taken upper solution, add 20mL Virahol and 10mL methyl alcohol in described upper solution, solid phase is reclaimed in centrifugation, and re-extract, centrifugal process promptly get the cadmium phosphide quanta point material 3 times.
Embodiment 11:
The preparation of a, cadmium presoma
Methyl ethyl diketone cadmium 0.62g and 15mL oleyl amine are placed the 25mL there-necked flask, extract volatilizable solvent under 100 ℃ of conditions out, at N
2Insulation reaction 20min obtains cadmium oleate solution in the atmosphere, yield 95.0%;
The preparation of b, cadmium phosphide quantum dot
The temperature of cadmium oleate solution is controlled at 150 ℃, down auxiliary in stream of nitrogen gas, feed PH
3Gas, PH
3Flow velocity is 2mL/min, carrier gas N
2Flow velocity is 30mL/min, N
2With PH
3Velocity ratio be 15: 1, insulation reaction 10min obtains the oleyl amine solution of cadmium phosphide quantum dot;
C, separation are purified
In the oleyl amine solution of cadmium phosphide quantum dot, add 20mL toluene, extracting and separating is left and taken upper solution, add 20mL Virahol and 10mL methyl alcohol in described upper solution, solid phase is reclaimed in centrifugation, and re-extract, centrifugal process promptly get the cadmium phosphide quanta point material 3 times.
Analyze explanation:
The present invention utilizes cheap phosphorus, chromium cpd to see Fig. 1 as the photo in kind of the resulting cadmium phosphide of presoma under ultra violet lamp of synthetic cadmium phosphide, among the figure from left to right, glow color is followed successively by blueness, green, yellow, orange, redness and region of ultra-red luminous, wherein the highest glow peak of sample of infraluminescence from a left side several the 6th be followed successively by 920nm, 1100nm, 1250nm, 1500nm; To the cadmium phosphide quanta point material of the present invention preparation adopt infrared-visible-ultraviolet absorption spectrum (Abs, Fig. 2 a, Fig. 2 b), fluorescence spectrum (PL, Fig. 3) and projection electron microscope (TEM, Fig. 4) etc. method is carried out phenetic analysis.The result shows that the cadmium phosphide nanocrystal is subsphaeroidal, and size is even, mean diameter 2nm-12nm, and this size can be by synthesis temperature and growth time regulation and control (Fig. 4); Increase along with cadmium phosphide quantum dot mean sizes, it is in ultraviolet arrives infrared SPECTRAL REGION, successive absorption peak (Fig. 2 a can appear, Fig. 2 b), its corresponding photoluminescence peak also changes along with absorption peak, thereby be implemented in luminous (Fig. 3) in the 460nm-1500nm scope, analysis revealed should the series glow peak be moved back by the interband of cadmium phosphide and is formed; Measure the luminescent lifetime (τ of ruddiness to infrared light
1/2) change between tens microseconds in hundreds of nanoseconds, and increase along with the increase of emission wavelength, show that the cadmium phosphide quantum dot is a kind of light-storing material of superior super twilight sunset.
Claims (6)
1. the preparation method of a low-cost cadmium phosphide quanta point material is characterized in that operating according to the following steps:
A, the Cadmium oxide of 2mmol and the longer chain fatty acid of 4mmol are joined in the there-necked flask that contains the 15mL octadecylene, in nitrogen atmosphere,, obtain the soap solution of cadmium in 260-280 ℃ of insulation reaction 20 minutes; Or the methyl ethyl diketone cadmium of 2mmol is dissolved in the 10-20mL organic amine, at N
2Be heated to 80-150 ℃ in the atmosphere, obtain the organic amine solution of methyl ethyl diketone cadmium;
The temperature of the soap solution of b, cadmium that step a is obtained is controlled at 60-320 ℃, and is down auxiliary in stream of nitrogen gas, feeds PH
3Gas, N
2With PH
3Velocity ratio be 1-15: 1, insulation reaction 2-180min obtains the octadecylene solution of cadmium phosphide quantum dot; Or the temperature of the organic amine solution of the methyl ethyl diketone cadmium that step a is obtained is controlled at 80-150 ℃, and is down auxiliary in stream of nitrogen gas, feeds PH
3Gas, N
2With PH
3Velocity ratio be 1-15: 1, insulation reaction 2-180min obtains the organic amine solution of cadmium phosphide quantum dot;
C, in the organic amine solution of the octadecylene solution of the cadmium phosphide quantum dot that step b obtains or cadmium phosphide quantum dot, add 20mL toluene, extracting and separating is left and taken upper solution, in described upper solution, add 20mL Virahol and 10mL methyl alcohol, solid phase is reclaimed in centrifugation, and re-extract, centrifugal process promptly get the cadmium phosphide quanta point material 3-5 time.
2. preparation method according to claim 1 is characterized in that: described cadmic compound is Cadmium oxide, cadmium acetate or methyl ethyl diketone cadmium.
3. preparation method according to claim 1 is characterized in that: described longer chain fatty acid is meant that carbon atom number is not less than 12 saturated or unsaturated fatty acids in the main chain.
4. preparation method according to claim 3 is characterized in that: described longer chain fatty acid is lauric acid, myristic acid, palmitinic acid, physetoleic acid, oleic acid, stearic acid, Palmiticacid, eicosanoic acid, mountain Yu acid or cerinic acid.
5. preparation method according to claim 1 is characterized in that: described organic amine is that carbon atom number is not less than 6 saturated or unsaturated fatty acids amine in the main chain.
6. preparation method according to claim 5 is characterized in that: described organic amine is an oleyl amine.
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| CN101294073A (en) * | 2008-06-12 | 2008-10-29 | 上海交通大学 | Indium phosphide fluorescence quantum pot synthesizing method |
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| SHIDING MIAO ET AL.: "Synthesis and Characterization of Cadmium Phosphide Quantum Dots Emitting in the Visible Red to Near-Infrared", 《J. AM. CHEM. SOC.》 * |
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| CN103936056B (en) * | 2014-05-07 | 2016-06-15 | 吉林大学 | A kind of preparation method of cadmium phosphide quantum dot |
| CN103936069A (en) * | 2014-05-07 | 2014-07-23 | 吉林大学 | Preparation method of cadmium arsenide quantum dots |
| CN103936056A (en) * | 2014-05-07 | 2014-07-23 | 吉林大学 | Preparation method of cadmium phosphide quantum dots |
| CN103937495A (en) * | 2014-05-07 | 2014-07-23 | 吉林大学 | Preparation method of cadmium phosphide semiconductor nanocluster |
| CN103936069B (en) * | 2014-05-07 | 2015-10-21 | 吉林大学 | The preparation method of a kind of Cadmium arsenide quantum dot |
| CN103936068B (en) * | 2014-05-07 | 2015-10-21 | 吉林大学 | The preparation method of a kind of Cadmium arsenide semiconductor cluster |
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