CN101844751B - Method for preparing lead selenide nanocrystals - Google Patents
Method for preparing lead selenide nanocrystals Download PDFInfo
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- CN101844751B CN101844751B CN2010101799973A CN201010179997A CN101844751B CN 101844751 B CN101844751 B CN 101844751B CN 2010101799973 A CN2010101799973 A CN 2010101799973A CN 201010179997 A CN201010179997 A CN 201010179997A CN 101844751 B CN101844751 B CN 101844751B
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- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/04—Binary compounds including binary selenium-tellurium compounds
Abstract
The invention discloses a method for preparing lead selenide nanocrystals. The method comprises the following steps of: putting selenium powder in a container; removing the air from the container and filling the container with inert gas; adding alkylamine which has a long chain with a boiling point of over 180 DEG C into the container; fully stirring and heating the selenium powder and the ammonia to perform full reaction so as to form ligand; adding lead chloride into the alkylamine which has the long chain with the boiling point of over 180 DEG C, fully stirring the mixture, vacuuming the container and then heating the mixture of the lead chloride and ammonia to fully dissolve the lead chloride in the ammonia; and injecting the mixture of selenium powder into the mixture of lead chloride to perform reaction so as to obtain the lead selenide nanocrystalline particles.
Description
Technical field
The invention belongs to solvent synthetic chemistry and nano semiconductor material fabricating technology field, relate to a kind of method that is prepared into of lead selenide nanocrystals.
Background technology
Lead selenide has caused people's extensive concern as a kind of important semiconductor material.It is that typical IV～VI family has the direct band-gap semicondictor of cube sodium chloride type structure, and energy gap is very little, and spectral absorption is arranged in infrared to visible region, has significant infrared electric conductivity matter.Because energy gap is narrow, lead selenide can be used for producing light detector, photoresistor, optical transmitting set.Keeping under the constant situation of other optical property, employing lead selenide nanocrystals (also being known as quantum dot) can controllably be regulated energy gap, thereby satisfies the demand of various devices better.At present, lead selenide nanocrystals is considered in fields such as photoelectronics, biophysics, fluorescence microscopy, important application prospects is arranged.
The a variety of methods that prepare lead selenide nanocrystals have been arranged at present.Comprise hydrothermal method, microwave method, sonochemical method, photochemical method, chemical radiation etc.But more than desired method preparation condition strict, complex operation, time remaining is long, cost is high, or it is unsatisfactory to prepare effect.Solvent-thermal method is a kind of method that is most commonly used to prepare lead selenide nanocrystals at present, and its preparation time is short, prepares effective.In calendar year 2001, and people such as Murray (IBM J.Res.Dev.2001,45, reported with solvent method and synthesized lead selenide nanocrystals 47-55.) that after this much human has been synthesized the lead selenide nanocrystals of various different sizes and shape with this method the first time.But the shortcoming of this method is: (1), to use different solvents such as oleic acid in the building-up process, 18 rare and tri octyl phosphines.(2), solvent expensive and environmental pollution are serious.(3), operating process is loaded down with trivial details relatively.
Chinese invention patent application 200810069242.0 discloses the preparation method of a kind of selenide and telluride nano crystal material, can be used for preparing lead selenide.This method is: replace water or organic solvent in the existing hydrothermal/solvent process for thermosynthesizing with fused composite alkali metal oxyhydroxide, synthesize at normal pressure and the 100-300 ℃ of following chemical reaction that passes through.
Chinese invention patent 200510119122.3 provides a kind of preparation method of aqueous phase lead selenide nano material.This method adopts plumbic acetate and selenourea to be respectively plumbous source and selenium source; To dredge guanidine-acetic acid, thin basic propionic acid, halfcystine, thioglycerol, thin basic ethanol etc. is coating; Through reaction under 60 ℃～180 ℃ conditions 15 minutes～90 minutes, obtain a kind of aqueous phase lead selenide nano material.
Summary of the invention
The present invention provides a kind of method with the simply synthetic lead selenide nanocrystals of solvent-thermal method.
The preparation method that the present invention prepares lead selenide nanocrystals is:
A, selenium powder is put into container; Drive away the air in the container and charge into rare gas element; Adding 0.03125～0.125 milliliter ratio in every milligram of selenium powder, slowly to add the long-chain boiling point be the alkylamine more than 180 ℃, through fully after the stirring selenium powder amine mixed solution being heated to 185 ℃～220 ℃, makes mixed solution slowly become transparent liquid by black suspension; Be incubated again, make selenium powder and amine fully act on the formation settled solution;
B, in another container, adding 2.248～18.000 milliliters ratio in every gram lead chloride, slowly to add the long-chain boiling point be the alkylamine more than 180 ℃; Through fully stirring; And vacuumize that (vacuum tightness reaches 0.07MPa～0.1MPa); After again lead chloride amine mixed solution being heated to 150 ℃～160 ℃; Be incubated after feeding rare gas element continued is warmed up to 190 ℃～240 ℃ in container again,, promote lead chloride fully dissolving in amine fully to remove the moisture and other lower-boiling impurity that possibly exist in the amine aqueous solution;
C, be the selenium powder mixed solution to be injected in the lead chloride mixed solution in 10: 1～1: 2, after reaction, be cooled fast to room temperature, add the 10mL chloroform by the ratio of lead chloride and selenium amount of substance.In reaction system, extraordinarily go into ethanol subsequently, the lead selenide nanocrystals solids precipitation is separated out, after solid-liquid separation, carry out drying treatment, obtain the lead selenide nanocrystals particle by 2 of reaction soln volume.
It is that alkylamine more than 180 ℃ is meant oleyl amine or cetylamine or stearylamine or amino dodecane or 1,6 hexanediamine etc. that the present invention prepares long-chain boiling point used in the method for lead selenide nanocrystals, and solid amine can be about to the amine heating earlier in concrete the use, make it become liquid state.
The present invention prepares in the method for lead selenide nanocrystals should eliminate the air in the reactant, and the agents useful for same water cut is not higher than 0.05% of total mass, and test shows available pattern and lead selenide nanocrystals of uniform size under such condition.
The present invention prepares in the process of lead selenide nanocrystals, after each corresponding solution temperature reaches requirement, should guarantee that the rangeability of temperature of reaction should be less than ± 1 ℃.Test shows can obtain the uniform nanocrystal of particle diameter like this.Experiment shows range of temperature greater than ± 1 ℃, can cause particle size distribution range to increase.
The present invention is when the preparation lead selenide nanocrystals, and described reacting material ratio can be different, but should guarantee that the lead chloride strength of solution should be greater than 2.25 grams per milliliters.If concentration is greater than this numerical value, consequently the part lead chloride can be separated out and attached on the wall of container, causes actual material ratio not meet theoretical value and influences the carrying out of reaction.
The present invention adopts vacuum drying oven when the lead selenide nanocrystals particle is carried out drying treatment in the process of preparation lead selenide nanocrystals, the temperature of vacuum drying oven is 30 ℃～80 ℃.Test shows, when the loft drier temperature is lower than 30 ℃, the time that lead selenide is dried is relatively long, can cause lead selenide nanocrystalline oxidized and be higher than 80 ℃.
When relevant experiment the present invention prepares lead selenide nanocrystals; The mixed solution of described lead chloride and amine is heated to and should be incubated half a hour to one hour behind the preset temperature; Can fully make the reaction of amine and lead chloride generate title complex like this; Selenium powder fully is dissolved in the amine, helps reaction thereafter.
Among the preparation method of lead selenide nanocrystals of the present invention, its related technical parameters is controlled at: 40 milligrams of selenium powders join in 2.5 milliliters the oleyl amine, and temperature rises to 200 ℃; Logical argon gas continued to be warmed up to 220 ℃ after 556 milligrams lead chloride joined and under vacuum condition, is warmed up to 160 ℃ in 5 milliliters of oleyl amines; Under 220 ℃, selenium and oleyl amine mixed solution are injected lead chloride and oleyl amine mixed solution; Reaction times is 40 minutes, has best effect.
The present invention not only makes tensio-active agent but also make lead chloride and the complexing agent of selenium powder with amine, can guarantee the homodisperse of two kinds of reactants.At high temperature, lead ion and plasma selenium can react, and after forming the lead selenide nano particle, amine can wrap the effect that the lead selenide nano particle reaches stable dispersion.
The present invention has following advantage: it is simple, cheap 1) to prepare the used solvent of lead selenide nanocrystals, economy; Compare with the technology that has other now, the present invention is environmental protection more, does not produce too much pollution.2) preparation technology's flow process is simple, does not need severe condition such as HTHP, and suitable continuous production.3) adopt the present invention, also can be through the process of CONTROL PROCESS, the form of control product for example can obtain spherical or cube shaped nanocrystal.
Description of drawings
Accompanying drawing 1,3,5,6 is the transmission electron microscope photo of product of the present invention, Fig. 2,4,7 is the near infrared absorption figure of product of the present invention.Fig. 8,9,10 be product of the present invention X-ray powder diffraction figure wherein:
Fig. 1 be with oleyl amine as solvent and reactant, the ratio of the amount of substance of lead chloride and selenium powder is 2: 1, temperature of reaction is 220 ℃, the reaction times is 30 seconds lead selenide nanocrystals particulate transmission electron microscope photo.
Fig. 2 be with oleyl amine as solvent and reactant, the ratio of the amount of substance of lead chloride and selenium powder is 2: 1, temperature of reaction is 220 ℃.Reaction times is 30 seconds lead selenide nanocrystals particulate near infrared absorption figure.
Fig. 3 be with oleyl amine as solvent and reactant, the ratio of the amount of substance of lead chloride and selenium powder is 2: 1, temperature of reaction is 220 ℃, the reaction times is 1 minute lead selenide nanocrystals particulate transmission electron microscope photo.
Fig. 4 be with oleyl amine as solvent and reactant, the ratio of the amount of substance of lead chloride and selenium powder is 2: 1, temperature of reaction is 220 ℃.Reaction times is 1 minute lead selenide nanocrystals particulate near infrared absorption figure.
Fig. 5 be with oleyl amine as solvent and reactant, the ratio of the amount of substance of lead chloride and selenium powder is 2: 1, temperature of reaction is 220 ℃, the reaction times is 40 minutes lead selenide nanocrystals particulate transmission electron microscope photo.
Fig. 6 be with oleyl amine as solvent and reactant, the ratio of the amount of substance of lead chloride and selenium powder is 2: 1, temperature of reaction is 220 ℃, the reaction times is 40 minutes lead selenide nanocrystals particulate high-resolution-ration transmission electric-lens photo.
Fig. 7 be with oleyl amine as solvent and reactant, the ratio of the amount of substance of lead chloride and selenium powder is 2: 1, temperature of reaction is 220 ℃.Reaction times is 40 minutes lead selenide nanocrystals particulate near infrared absorption figure.
Fig. 8 be with oleyl amine as solvent and reactant, the ratio of the amount of substance of lead chloride and selenium powder is 2: 1, temperature of reaction is 220 ℃.Reaction times is 40 minutes lead selenide nanocrystals particulate X-ray powder diffraction figure.
Fig. 9 be with amino dodecane as solvent and reactant, the ratio of the amount of substance of lead chloride and selenium powder is 4: 1, temperature of reaction is 220 ℃.Reaction times is 40 minutes lead selenide nanocrystals particulate X-ray powder diffraction figure.
Figure 10 be with 1,6 hexanediamine as solvent and reactant, the ratio of the amount of substance of lead chloride and selenium powder is 4: 1, temperature of reaction is 220 ℃.Reaction times is 40 minutes lead selenide nanocrystals particulate X-ray powder diffraction figure.
Embodiment
Embodiment one
The concrete preparation process of this enforcement row is following:
A, at first gets 80 milligrams of selenium powders and puts into its outer two mouthfuls of flasks that cooling conditions is arranged, and drives away the flask air, charges into argon gas.
B, inject 5 milliliters of oleyl amines, stir with magneton with syringe.
C, heat above-mentioned selenium powder mixed solution to 220 ℃ with oil bath, mixed solution slowly becomes transparent light red orange liquid by black suspension, keeps 220 ℃ more than half hour.
D, secondly gets 556 milligrams of lead chlorides and puts into 50 milliliters of two mouthfuls of flasks that have water of condensation, injects 5 milliliters of oleyl amines with syringe, stirs with magneton, vacuumizes half a hour.
E, heat above-mentioned lead chloride mixing solutions to 160 ℃ with oil bath after, feed the argon gas continued and be warmed up to 220 ℃, hold liquid and become white emulsion, keep 220 ℃ more than half a hour.
F, be injected into the selenium powder mixed solution in the lead chloride mixed solution then, react and be cooled fast to room temperature after 30 seconds, add the 10mL chloroform.
The lead selenide nanocrystals particle that h, an amount of ethanol sedimentation of adding prepare, and spinning in supercentrifuge.
G, sample is dry in vacuum drying oven, temperature is 30 ℃, drying time is 12 hours, finally obtains the lead selenide nanocrystals particle of black.
Made sample is distributed in the chloroformic solution test transmission electron microscope again sees Fig. 1, visible by Fig. 1, resulting lead selenide nanocrystals particle is spherical, and size is about about 6 nanometers.The near infrared absorption spectrum is seen Fig. 2, and its absorption peak position is about about 1800 nanometers.
Embodiment two
The concrete preparation process of this enforcement row is following:
A, at first gets 80 milligrams of selenium powders and puts into its outer two mouthfuls of flasks that cooling conditions is arranged, and drives away the flask air, charges into argon gas.
B, inject 5 milliliters of oleyl amines, stir with magneton with syringe.
C, heat above-mentioned selenium powder mixed solution to 220 ℃ with oil bath, mixed solution slowly becomes transparent light red orange liquid by black suspension, keeps 220 ℃ more than half hour.
D, secondly gets 556 milligrams of lead chlorides and puts into 50 milliliters of two mouthfuls of flasks that have water of condensation, injects 5 milliliters of oleyl amines with syringe, stirs with magneton, vacuumizes half a hour.
E, heat above-mentioned lead chloride mixing solutions to 160 ℃ with oil bath after, feed the argon gas continued and be warmed up to 220 ℃, hold liquid and become white emulsion, keep 220 ℃ more than half a hour.
F, be injected into the selenium powder mixed solution in the lead chloride mixed solution then, react and be cooled fast to room temperature after 1 minute, add the 10mL chloroform.
The lead selenide nanocrystals particle that h, an amount of ethanol sedimentation of adding prepare, and spinning in supercentrifuge.
G, sample is dry in vacuum drying oven, temperature is 40 ℃, drying time is 18 hours, finally obtains the lead selenide nanocrystals particle of black.
Made sample is distributed in the chloroformic solution test transmission electron microscope again sees Fig. 3, test shows that after the reaction times was 1 minute, particle is mostly to be cube.And size is about about 10 nanometers.Its near infrared absorption spectrum is seen Fig. 4, and its absorption peak position is about about 1900 nanometers.
Embodiment three
The concrete preparation process of this enforcement row is following:
A, at first gets 80 milligrams of selenium powders and puts into its outer two mouthfuls of flasks that cooling conditions is arranged, and drives away the flask air, charges into argon gas.
B, inject 5 milliliters of oleyl amines, stir with magneton with syringe.
C, heat above-mentioned selenium powder mixed solution to 220 ℃ with oil bath, mixed solution slowly becomes transparent light red orange liquid by black suspension, keeps 220 ℃ more than half hour.
D, secondly gets 556 milligrams of lead chlorides and puts into 50 milliliters of two mouthfuls of flasks that have water of condensation, injects 5 milliliters of oleyl amines with syringe, stirs with magneton, vacuumizes half a hour.
E, heat above-mentioned lead chloride mixing solutions to 160 ℃ with oil bath after, feed the argon gas continued and be warmed up to 220 ℃, hold liquid and become white emulsion, 220 ℃ more than half a hour.
F, be injected into the selenium powder mixed solution in the lead chloride mixed solution then, react and be cooled fast to room temperature after 40 minutes, add the 10mL chloroform.
The lead selenide nanocrystals particle that h, an amount of ethanol sedimentation of adding prepare, and spinning in supercentrifuge.
G, sample is dry in vacuum drying oven, temperature is 50 ℃, drying time is 24 hours, finally obtains the lead selenide nanocrystals particle of black.
Made sample is distributed in the chloroformic solution test transmission electron microscope again referring to Fig. 5 and Fig. 6, but after the reaction times was 40 minutes, particle diameter was a cube, size is about 13 nanometers.Its near infrared absorption spectrum is seen Fig. 7, and its absorption peak position is about about 2000 nanometers.Again with prepared product repeatedly through detecting with x-ray powder diffraction instrument (XRD) after chloroform and the washing with alcohol, diffraction spectrogram such as Fig. 8, contrasting the confirmation product with the XRD spectra of standard P bSe really is that PdSe is nanocrystalline.
Embodiment four
The concrete preparation process of this enforcement row is following:
A, at first gets the amino dodecane of 40 milligrams of selenium powders and 2g and puts into its outer two mouthfuls of flasks that cooling conditions is arranged, and drives away the flask air, charges into argon gas.
B, heat above-mentioned selenium powder mixture to 220 ℃ with oil bath, begin to dissolve at 80 ℃ of left and right sides amino dodecanes, stir with magneton, mixed solution slowly becomes transparent light safran liquid by black suspension, keeps this temperature more than half hour.
D, secondly gets 556 milligrams of lead chlorides and 3g amino dodecane and puts into 50 milliliters of two mouthfuls of flasks that have water of condensation.
C, heat above-mentioned lead chloride mixture to 160 ℃ with oil bath after, feed the argon gas continued with magneton and be warmed up to 220 ℃, hold liquid and become white emulsion, keep this temperature more than half a hour.
D, be injected into the selenium powder mixed solution in the lead chloride mixed solution then, react and be cooled fast to room temperature after 40 minutes, add the 10mL chloroform.
The lead selenide nanocrystals particle that h, an amount of ethanol sedimentation of adding prepare, and spinning in supercentrifuge.
G, sample is dry in vacuum drying oven, temperature is 50 ℃, drying time is 24 hours, finally obtains the lead selenide nanocrystals particle of black.
With prepared product repeatedly through detecting with x-ray powder diffraction instrument (XRD) after chloroform and the washing with alcohol, diffraction spectra such as Fig. 9, contrasting the confirmation product with the XRD spectra of standard P bSe really is that PdSe is nanocrystalline.
Embodiment five
The concrete preparation process of this enforcement row is following:
A, at first gets 40 milligrams of selenium powders and puts into its outer two mouthfuls of flasks that cooling conditions is arranged, and drives away the flask air, charges into argon gas.
B, inject 5 milliliter of 1,6 hexanediamine, stir with magneton with syringe.
C, heat above-mentioned selenium powder mixed solution to 220 ℃ with oil bath, mixed solution slowly becomes transparent light safran liquid by black suspension, keeps 220 ℃ more than half hour.
D, secondly gets 556 milligrams of lead chlorides and puts into 50 milliliters of two mouthfuls of flasks that have water of condensation, injects 5 milliliter of 1,6 hexanediamine with syringe, stirs with magneton, vacuumizes half a hour.
E, heat above-mentioned lead chloride mixing solutions to 160 ℃ with oil bath after, feed the argon gas continued and be warmed up to 220 ℃, hold liquid and become white emulsion, keep 220 ℃ more than half a hour.
F, be injected into the selenium powder mixed solution in the lead chloride mixed solution then, react and be cooled fast to room temperature after 40 minutes, add the 10mL chloroform.
The lead selenide nanocrystals particle that h, an amount of ethanol sedimentation of adding prepare, and spinning in supercentrifuge.
G, sample is dry in vacuum drying oven, temperature is 50 ℃, drying time is 24 hours, finally obtains the lead selenide nanocrystals particle of black.
With prepared product repeatedly through detecting with x-ray powder diffraction instrument (XRD) after chloroform and the washing with alcohol, diffraction spectra such as Fig. 9, contrasting the confirmation product with the XRD spectra of standard P bSe really is that PdSe is nanocrystalline.
Claims (7)
1. the preparation method of a lead selenide nanocrystals is characterized in that:
A, selenium powder is put into container; Drive away the air in the container and charge into rare gas element; Adding 0.03125～0.125 milliliter ratio in every milligram of selenium powder, slowly to add the long-chain boiling point be the alkylamine more than 180 ℃; After fully stirring, selenium powder and amine mixed solution are heated to 185 ℃～220 ℃, are incubated again, make selenium powder and amine fully act on the formation settled solution;
B, in another container, adding 2.248～18.000 milliliters ratio in every gram lead chloride, slowly to add the long-chain boiling point be the alkylamine more than 180 ℃; Through fully stirring; And vacuumize, vacuum tightness reaches 0.07MPa～0.1MPa, again lead chloride and amine mixed solution are heated to 150 ℃～160 ℃ after; Be incubated after feeding rare gas element continued is warmed up to 190 ℃～240 ℃ in container again, so that lead chloride fully dissolving in amine;
C, be the selenium powder mixed solution to be injected in the lead chloride mixed solution in 10: 1～1: 2, keep solution temperature constant, reacted as required 0.1～60 minute by the ratio of lead chloride and selenium amount of substance; After finishing, the reaction back is cooled fast to room temperature; Add the 10mL chloroform, in reaction system, extraordinarily go into ethanol subsequently, the lead selenide nanocrystals solids precipitation is separated out by 2 of reaction soln volume; After solid-liquid separation, carry out drying treatment, obtain the lead selenide nanocrystals particle;
Described long-chain boiling point is that the alkylamine more than 180 ℃ is oleyl amine or cetylamine or stearylamine or amino dodecane or 1,6 hexanediamine.
2. the preparation method of a kind of lead selenide nanocrystals as claimed in claim 1 is characterized in that when the preparation lead selenide nanocrystals, should eliminating the air in the reaction, and the agents useful for same water cut is not higher than 0.05% of total mass.
3. the preparation method of a kind of lead selenide nanocrystals as claimed in claim 2 is characterized in that in the process of preparation lead selenide nanocrystals, after each corresponding solution temperature reaches requirement, should guaranteeing that the rangeability of temperature of reaction should be less than ± 1 ℃.
4. the preparation method of a kind of lead selenide nanocrystals as claimed in claim 3 is characterized in that the lead chloride strength of solution should be greater than 2.25 grams per milliliters when the preparation lead selenide nanocrystals.
5. the preparation method of a kind of lead selenide nanocrystals as claimed in claim 4; It is characterized in that in the process of preparation lead selenide nanocrystals; Adopt vacuum drying oven when the lead selenide nanocrystals particle is carried out drying treatment, the temperature of vacuum drying oven is 30 ℃～80 ℃.
6. the preparation method of a kind of lead selenide nanocrystals as claimed in claim 5 is characterized in that selenium powder and amine mixed solution and described lead chloride and amine mixed solution are heated to should be incubated half a hour to one hour behind the preset temperature.
7. the preparation method of a kind of lead selenide nanocrystals as claimed in claim 6 is characterized in that 40 milligrams of selenium powders join in 2.5 milliliters the amine, and temperature rises to 200 ℃; 556 milligrams lead chloride joins in 5 milliliters of amine, under vacuum condition, be warmed up to 160 ℃ after logical argon gas continue to be warmed up to 220 ℃, under 220 ℃, selenium and the injection of amine mixed solution be dissolved with the amine mixed solution of lead chloride, the reaction times is 40 minutes.
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