CN102718249A - Method for preparing CuInS2 nanocrystalline and CuInS2/ZnS core-shell structure nanocrystalline - Google Patents
Method for preparing CuInS2 nanocrystalline and CuInS2/ZnS core-shell structure nanocrystalline Download PDFInfo
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- CN102718249A CN102718249A CN2012101383384A CN201210138338A CN102718249A CN 102718249 A CN102718249 A CN 102718249A CN 2012101383384 A CN2012101383384 A CN 2012101383384A CN 201210138338 A CN201210138338 A CN 201210138338A CN 102718249 A CN102718249 A CN 102718249A
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Abstract
The invention discloses a method for preparing CuInS2 nanocrystalline and CuInS2/ZnS core-shell structure nanocrystalline, which is characterized in that stearic acid indium is reacted with cuprous iodide with the same mole in a mixed solution containing oleic acid, superfluous dodecanethiol and octadecene to obtain the CuInS2 nanocrystalline, a zinc stearate solution is added to obtain the CuInS2/ZnS core-shell structure nanocrystalline. The CuInS2 nanocrystalline and the CuInS2/ZnS core-shell structure nanocrystalline have the characteristics of homogeneous phase, low toxicity, good monodispersity, strong repeatability, wide spectrum coverage and high fluorescent quantum yield, wherein the fluorescent quantum yield of the CuInS2 nanocrystalline can reach as high as 8.7%; and the fluorescent quantum yield of the CuInS2/ZnS nanocrystalline can reach as high as 60%. The method of the invention has the advantages of easy available and stable raw materials, safe and convenient operation and no requirement of rigorous condition; thereby the laboratory large-scale preparation and industrial production of the CuInS2 nanocrystalline and CuInS2/ZnS core-shell structure nanocrystalline realize the possibility.
Description
Technical field
The invention belongs to field of inorganic nano material, be specifically related to CuInS
2The preparation method of nanocrystalline (quantum dot).The invention still further relates to CuInS
2The preparation method of/ZnS nano-crystal with core-shell structure (quantum dot)
Background technology
(quantum dots QDs) is three-dimensional limited, approximate globular inorganic semiconductor nanocrystal to quantum dot.Owing to the optical property of the nanocrystalline excellence of inorganic semiconductor, aspect fluorescent mark, attracted numerous scientists' research interest.For example, living microbe fluorescence imaging technology has become present most active subject direction.Regrettably, a little less than the fluorescence nano penetrativity of VISIBLE LIGHT EMISSION, limited its application aspect the living microbe fluorescence imaging.In order to overcome the problem a little less than the penetration power, a series of near-infrared quantum dots (750-900nm) are developed, mainly comprise II-VI (CdTe/CdSe, CdSe/ZnTe), IV-VI (PbS, PbSe), II-V (Cd
3P
2), but, cause environmental pollution easily because these quantum dots include Cd and the poisonous element of Pb.So, the CuInS of low toxicity
2Near-infrared quantum dots gradually becomes the focus of research.
CuInS
2Be direct band gap, bandwidth is the semiconductor nano of 1.45eV.Human Triple Pressed Stearic Acid indium such as Peng and neutralized verdigris are metal precursor, adopt the hot injection method of organic phase, have synthesized high quality, near infrared CuInS
2Nanocrystalline, but compound method is complicated, poor repeatability, the nanocrystalline fluorescence quantum yield of synthetic low (being lower than 3%); Human cuprous acetates such as Zhong and indium acetate have synthesized CuInS
2Nanocrystalline, but its emission peak maximum does not reach near infrared region at 740nm; Afterwards, people such as Li used cuprous iodide and indium acetate to be metal precursor based on the method the same with Zhong, had synthesized near infrared CuInS
2Nanocrystalline, but owing to there is not the reactive behavior of two metal precursors of balance, it is nanocrystalline to be homogeneous not, and system contains CuS and In
2S
3Impurity can't separate.
Summary of the invention
Technical problem to be solved by this invention provides a kind of CuInS
2Preparation of nano crystal, this method is easy and simple to handle, and raw material is easy to get, and reaction conditions is gentle, synthetic CuInS
2Nanocrystalline homogeneous phase, low toxicity, and monodispersity is good, and repeatability is strong, and fluorescence quantum yield is higher relatively.
Another technical problem to be solved by this invention provides a kind of CuInS
2/ ZnS nano-crystal with core-shell structure, the relative CuInS of fluorescence quantum yield
2Nanocrystalline had a further raising.
For solving above-mentioned first technical problem, technical scheme provided by the invention comprises the steps:
1) with amount of substance than putting into there-necked flask, under nitrogen atmosphere, in 140 for the indium acetate of 1:12 and Triple Pressed Stearic Acid
oC reaction 5 hours is cooled to room temperature, then through washing with acetone, filtration, vacuum-drying, gets Triple Pressed Stearic Acid indium crude product;
2) Triple Pressed Stearic Acid of the amount of substance of itself and 8 times of indium acetates in step 1) is put into there-necked flask, the same step 1) of other reaction conditions, reaction product grind to form Triple Pressed Stearic Acid indium powder after washing with acetone, filtration, vacuum-drying;
In the mixed solvent of the oleic acid that 3) will wait cuprous iodide and the Triple Pressed Stearic Acid indium powder of amount of substance to add to contain 200-500 μ l, the Dodecyl Mercaptan of 0.7-1.25ml and vaccenic acid, under nitrogen atmosphere, be warming up to 70
oC keeps 30-60min, is warming up to 200-250 then
oC reacted no more than 5 hours, was cooled to room temperature; It is dispersed in chloroform and the methyl alcohol mixed liquor, adds acetone precipitation then, spinning discards supernatant liquid, and throw out is taken out vacuum-drying, promptly gets CuInS
2Nanocrystalline.If preparation CuInS
2/ ZnS then in this step, need not be cooled to room temperature and carry out the centrifugal purification process, and directly carry out next step reaction.
Vaccenic acid does not have remarkable influence as the reaction solvent of body series for product performance, and its consumption does not have strict restriction yet, is preferably 10ml.
4) dropwise drip the Zinic stearas that is dissolved in tri octyl phosphine and vaccenic acid, kept 30 minutes, be cooled to room temperature then; It is dispersed in chloroform and the methyl alcohol mixed liquor, adds acetone precipitation, spinning; Discard supernatant liquid, throw out is taken out vacuum-drying, promptly get CuInS
2/ ZnS is nanocrystalline;
The amount of substance of cuprous iodide is than being 2-10:1 in the amount of substance of said Zinic stearas and the step 3).
The present invention prepares pulverous Triple Pressed Stearic Acid indium through two-step approach; And with ten Er Liu Chun ﹑ oleic acid and vaccenic acid mixed solvent (Dodecyl Mercaptan is simultaneously as the sulphur source of reacting) as Triple Pressed Stearic Acid indium and cuprous iodide reaction; Preferably balance the activity of Triple Pressed Stearic Acid indium and cuprous iodide, prepare homogeneous phase, low toxicity, monodispersity is good, the wave spectrum coverage is wide CuInS
2Nanocrystalline, the scope of its fluorescent emission peak position is 695-835nm, and fluorescence quantum yield is up to 8.7%; Through Passivation Treatment, synthetic CuInS
2The quantum yield of/ZnS nano-crystal with core-shell structure is greatly improved, and the scope of fluorescent emission peak position is 620-820nm, and fluorescence quantum yield is up to 60%.Adopt the present invention, raw material is easy to get stable, and simple and safe operation does not need exacting terms, makes laboratory mass preparation and even suitability for industrialized production become possibility.The quantum dot that obtains used methods such as uv-visible absorption spectra, fluorescence spectrum, high-resolution-ration transmission electric-lens, x-ray powder crystalline diffraction to characterize.
Description of drawings:
Fig. 1 is the Triple Pressed Stearic Acid indium (In (SA) of the present invention's preparation
3) infared spectrum;
Fig. 2 is the prepared CuInS of the present invention
2Nanocrystalline ability spectrogram;
Fig. 3 is the prepared 3-4nm CuInS that is of a size of of the present invention
2Nanocrystalline HRTEM picture;
Fig. 4 is the CuInS of different-grain diameter
2Nanocrystalline fluorescence (a) and uv-visible absorption spectroscopy (b);
Fig. 5 is the CuInS of different emission peaks
2Nanocrystalline quantum yield (a) and fluorescence lifetime collection of illustrative plates (b);
Fig. 6 is the prepared CuInS of the present invention
2And CuInS
2The X-ray powder diffraction figure that/ZnS is nanocrystalline;
Fig. 7 is with 3-4 nm CuInS
2The CuInS that nanocrystalline (a) makes for nuclear
2The HRTEM picture that/ZnS (b) is nanocrystalline.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is done further detailed explanation.
Implementation process of the present invention comprises following four steps:
1) with amount of substance than putting into there-necked flask, under nitrogen atmosphere, in 140 for the indium acetate of 1:12 and Triple Pressed Stearic Acid
oC reaction 5 hours is cooled to room temperature, then through washing with acetone, filtration, vacuum-drying, gets Triple Pressed Stearic Acid indium crude product;
2) Triple Pressed Stearic Acid of the amount of substance of itself and 8 times of indium acetates in step 1) is put into there-necked flask, the same step 1) of other reaction conditions, reaction product grind to form Triple Pressed Stearic Acid indium powder after washing with acetone, filtration, vacuum-drying;
In the mixed solvent of the oleic acid that 3) will wait cuprous iodide and the Triple Pressed Stearic Acid indium powder of amount of substance to add to contain 200-500 μ l, the Dodecyl Mercaptan of 0.7-1.25ml and vaccenic acid, under nitrogen atmosphere, be warming up to 70
oC keeps 30-60min, is warming up to 200-250 then
oC reacted no more than 5 hours, was cooled to room temperature; It is dispersed in chloroform and the methyl alcohol mixed liquor, adds acetone precipitation then, spinning discards supernatant liquid, and throw out is taken out vacuum-drying, promptly gets CuInS
2Nanocrystalline.If preparation CuInS
2/ ZnS then in this step, need not be cooled to room temperature and carry out the centrifugal purification process, and directly carry out next step reaction.
Vaccenic acid does not have remarkable influence as the reaction solvent of body series for product performance, and its consumption does not have strict restriction yet, is preferably 10ml.
4) dropwise drip the Zinic stearas that is dissolved in tri octyl phosphine and vaccenic acid, kept 30 minutes, be cooled to room temperature then; It is dispersed in chloroform and the methyl alcohol mixed liquor, adds acetone precipitation, spinning; Discard supernatant liquid, throw out is taken out vacuum-drying, promptly get CuInS
2/ ZnS is nanocrystalline;
The amount of substance of cuprous iodide is than being 2-10:1 in the amount of substance of said Zinic stearas and the step 3).
1) takes by weighing the In (Ac) of 2.92g
3Put into there-necked flask with 95% the Triple Pressed Stearic Acid of 36g, under nitrogen atmosphere, in 140
o C reaction 5 hours is cooled to room temperature, uses washing with acetone then three times, after filtration, vacuum-drying, gets Triple Pressed Stearic Acid indium crude product;
2) 95% the Triple Pressed Stearic Acid of itself and 24g is put into there-necked flask, the same step 1) of other reaction conditions, reaction product grind to form Triple Pressed Stearic Acid indium powder after washing with acetone, filtration, vacuum-drying;
3) the Triple Pressed Stearic Acid indium powder of the CuI of 0.0191g and 0.1g is dissolved in the mixed solvent of vaccenic acid of Dodecyl Mercaptan and 10ml of the oleic acid that contains 210 μ l, 1 ml, under nitrogen atmosphere, is warming up to 70
oC kept 45 minutes, was warming up to 225 then
oC reacts 55 minutes (and taking a sample to 5,10,20,30,40,50 minutes in reaction respectively), is cooled to room temperature; It is dispersed in the chloroform and methyl alcohol mixed liquor of 5ml, adds the acetone of 30ml again, spinning; Throw out is taken out, and vacuum-drying can obtain CuInS
2Nanocrystalline.
As can beappreciated from fig. 1, Triple Pressed Stearic Acid (SA) is at 1715cm
-1The charateristic avsorption band at place become on the spectrogram of Triple Pressed Stearic Acid indium very a little less than, this spectrum peak is-in the COOH group-C=O-vibration peak, explain that Triple Pressed Stearic Acid has been converted into the Triple Pressed Stearic Acid indium, and the 1540cm that occurs from Triple Pressed Stearic Acid indium (In (SA) 3) spectrogram
-1The absorption peak at place, promptly the COO-vibration peak can further obtain proof.Contain Cu, In, three kinds of elements of S the synthetic product from can spectrogram can finding out of Fig. 2.Can find out the CuInS that the embodiment of the invention obtains from Fig. 3
2The nanocrystalline 3-4nm that is of a size of.The CuInS that obtains when the step 3) reaction times is respectively 5,10,20,30,40,50,55 minutes among the embodiment 1
2Nanocrystalline fluorescence and uv-visible absorption spectroscopy are seen Fig. 4, can know synthetic CuInS from Fig. 4
2The scope of nanocrystalline fluorescent emission peak position is 695-835nm, can know that from Fig. 5 its fluorescence quantum yield is up to 8.7%.
Embodiment 2
1) takes by weighing 2.92gIn (Ac)
3Put into there-necked flask with 95% the Triple Pressed Stearic Acid of 36g, under nitrogen atmosphere, in 140
o C reaction 5 hours is cooled to room temperature, uses washing with acetone then three times, filters and obtains the Triple Pressed Stearic Acid indium, after the vacuum-drying, gets Triple Pressed Stearic Acid indium crude product;
2) 95% the Triple Pressed Stearic Acid of itself and 24g is put into there-necked flask, the same step 1) of other reaction conditions, reaction product grind to form Triple Pressed Stearic Acid indium powder after washing with acetone, filtration, vacuum-drying;
3) 95% the Triple Pressed Stearic Acid indium of the CuI of 0.0191g and 0.1g is dissolved in the mixed solvent of vaccenic acid of Dodecyl Mercaptan and 10ml of the oleic acid that contains 210 μ l, 1ml, under nitrogen atmosphere, is warming up to 70
oC kept 45 minutes, was warming up to 225 then
oC reacted 30 minutes;
4) the 0.316g Zinic stearas is dissolved in the mixed solvent of trioctylphosphine phosphorus of 2ml vaccenic acid and 0.5ml, in 10-20 minute, dropwise splashes into, kept 30 minutes with syringe; Be cooled to room temperature then, it is dispersed in the chloroform and methyl alcohol mixed liquor of 5 ml, add the acetone of 30ml again; Spinning; Throw out is taken out, and vacuum-drying can obtain CuInS
2Nanocrystalline, its quantum yield has reached 60%.
Fig. 6 is respectively gained CuInS
2Nanocrystalline and CuInS
2The X-ray powder diffraction figure that/ZnS is nanocrystalline is with the data consistent of people such as Peng report (R.G. Xie, M. Rutherford, X.G. Peng, J. Am. Chem. Soc. 131 (2009) 5691).Fig. 7 is respectively synthetic CuInS
2Nanocrystalline (a) and with this big or small CuInS
2Nanocrystalline for the CuInS of nucleosynthesis
2The high-resolution electron microscopy figure that/ZnS (b) core-shell type nano is brilliant finds from Fig. 7, and the nanocrystalline particle diameter after the involucrum becomes big, and being synthesized of the brilliant success of core-shell type nano is described.
Under the constant situation of other conditions, the temperature of reaction and the reaction times of the step 3) of contriver through changing embodiment 1 and embodiment 2, find when temperature of reaction be 200
oC, the reaction times when reaching the highest fluorescent emission peak position (835nm) is 5 hours, and temperature of reaction is 250
oC, the reaction times when reaching minimum fluorescent emission peak position (695nm) is 2 minutes.
Under the constant situation of other conditions, the contriver is through changing the amount of Zinic stearas among the embodiment 2, when the add-on of finding Zinic stearas is 0.126g, and the CuInS of preparation
2The nanocrystalline quantum yield of/ZnS is 32%, when the add-on of Zinic stearas is 0.632g, and the CuInS of preparation
2The nanocrystalline quantum yield of/ZnS is 45%, and add-on is 0.316 o'clock, the CuInS of preparation
2The nanocrystalline quantum yield of/ZnS reaches 60%.
Claims (2)
1. CuInS
2Preparation of nano crystal is characterized in that: may further comprise the steps:
1) with amount of substance than putting into there-necked flask, under nitrogen atmosphere, in 140 for the indium acetate of 1:12 and Triple Pressed Stearic Acid
oC reaction 5 hours is cooled to room temperature, then through washing with acetone, filtration, vacuum-drying, gets Triple Pressed Stearic Acid indium crude product;
2) Triple Pressed Stearic Acid of the amount of substance of itself and 8 times of indium acetates in step 1) is put into there-necked flask, the same step 1) of other reaction conditions, reaction product grind to form Triple Pressed Stearic Acid indium powder after washing with acetone, filtration, vacuum-drying;
In the mixed solvent of the oleic acid that 3) will wait cuprous iodide and the Triple Pressed Stearic Acid indium powder of amount of substance to add to contain 200-500 μ l, the Dodecyl Mercaptan of 0.7-1.25ml and vaccenic acid, under nitrogen atmosphere, be warming up to 70
oC keeps 30-60min, is warming up to 200-250 then
oC reacted no more than 5 hours, was cooled to room temperature; It is dispersed in chloroform and the methyl alcohol mixed liquor, adds acetone precipitation then, spinning discards supernatant liquid, and throw out is taken out vacuum-drying, promptly gets CuInS
2Nanocrystalline.
2. CuInS
2The preparation method of/ZnS nano-crystal with core-shell structure is characterized in that: at preparation CuInS
2The 3rd nanocrystalline step, be warming up to 200-250
oC reacted after 0-55 minute, dropwise dripped the Zinic stearas that is dissolved in tri octyl phosphine and vaccenic acid, kept 30 minutes; Be cooled to room temperature then, it is dispersed in chloroform and the methyl alcohol mixed liquor, add acetone precipitation, spinning; Discard supernatant liquid, throw out is taken out vacuum-drying, promptly get CuInS
2/ ZnS is nanocrystalline;
The amount of substance of said Zinic stearas is 2-10:1 with the amount of substance of cuprous iodide ratio.
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CN102951676A (en) * | 2012-11-22 | 2013-03-06 | 温州大学 | One-step synthetic preparation method of CuInS2 nanowires |
CN103215034A (en) * | 2013-03-15 | 2013-07-24 | 河南大学 | Preparation method of high-quality CuInZnxS2+x/ZnS (0 <=x<=1) semiconductor nanocrystalline with core-shell structure |
CN104894635A (en) * | 2015-04-27 | 2015-09-09 | 武汉理工大学 | Size-controlled copper antimony sulfur nano crystal material and preparation method thereof |
WO2016179920A1 (en) * | 2015-05-14 | 2016-11-17 | 中国科学院广州能源研究所 | CuInS2/In2S3/ZnS FLUORESCENT QUANTUM DOT WITH DOUBLE-LAYER CORE-SHELL STRUCTURE AND PREPARATION METHOD THEREFOR |
CN108328647A (en) * | 2018-02-28 | 2018-07-27 | 武汉理工大学 | A kind of wurtzite structure CuInS2Nanocrystalline preparation method |
CN111819267A (en) * | 2018-02-15 | 2020-10-23 | 国立大学法人大阪大学 | Core-shell semiconductor nanoparticle, method for producing same, and light-emitting device |
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CN102277159A (en) * | 2011-06-13 | 2011-12-14 | 天津大学 | CuInS2/ZnS core-shell structured quantum dot and preparation method thereof |
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CN102951676B (en) * | 2012-11-22 | 2014-07-16 | 温州大学 | One-step synthetic preparation method of CuInS2 nanowires |
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WO2016179920A1 (en) * | 2015-05-14 | 2016-11-17 | 中国科学院广州能源研究所 | CuInS2/In2S3/ZnS FLUORESCENT QUANTUM DOT WITH DOUBLE-LAYER CORE-SHELL STRUCTURE AND PREPARATION METHOD THEREFOR |
US10563123B2 (en) | 2015-05-14 | 2020-02-18 | Guangzhou Institute Of Energy Conversion, Chinese Academy Of Sciences | CuInS2/In2S3/ZnS fluorescent quantum dot with double-layer core-shell structure and preparation method thereof |
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CN108328647A (en) * | 2018-02-28 | 2018-07-27 | 武汉理工大学 | A kind of wurtzite structure CuInS2Nanocrystalline preparation method |
CN108328647B (en) * | 2018-02-28 | 2020-04-10 | 武汉理工大学 | Wurtzite structure CuInS2Method for preparing nanocrystalline |
CN115340863A (en) * | 2022-06-29 | 2022-11-15 | 河北大学 | Near-infrared core-shell structure quantum dot CuInS 2 Method for synthesizing/ZnS |
CN115340863B (en) * | 2022-06-29 | 2023-11-14 | 河北大学 | Near infrared core-shell structure quantum dot CuInS 2 Method for synthesizing ZnS |
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