CN103936057A - Preparation method of cadmium sulfide quantum dots with controllable sizes - Google Patents

Preparation method of cadmium sulfide quantum dots with controllable sizes Download PDF

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CN103936057A
CN103936057A CN201410130418.4A CN201410130418A CN103936057A CN 103936057 A CN103936057 A CN 103936057A CN 201410130418 A CN201410130418 A CN 201410130418A CN 103936057 A CN103936057 A CN 103936057A
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CN103936057B (en
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康燕
佘厚德
魏娟娟
万新磊
雷自强
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Northwest Normal University
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Abstract

The invention relates to a preparation method of cadmium sulfide quantum dots with controllable size. The preparation method comprises the following steps: (1) adding cadmium nitrate tetrahydrate and sublimed sulfur to an oleylamine solution, and uniformly mixing so as to obtain a mixed solution; stirring the mixed solution at a room temperature, feeding inert gas argon, heating under the protection of the inert gas argon, and carrying out heat preservation at the temperature so as to obtain a yellow transparent mixed solution; heating the yellow transparent mixed solution in the presence of the inert gas argon, then carrying out heat preservation at the temperature, and naturally cooling to a room temperature so as to obtain a cooling solution; (2) adding absolute ethyl alcohol to the cooling solution so as to separate out yellow precipitates, and carrying out supersonic centrifugation so as to obtain a yellow precipitates and reaction mother liquor; centrifugally washing the precipitates by using an absolute ethyl alcohol and normal hexane mixed solution, and drying in vacuum until the weight is constant so as to obtain yellow powdery cadmium sulfide quantum dots with different sizes. The preparation method is simple, relatively low in cost and less in environmental pollution.

Description

The preparation method of the cadmiumsulfide quantum dot that a kind of size is controlled
Technical field
The present invention relates to the preparing technical field of semi-conductor amount point, relate in particular to the preparation method of the controlled cadmiumsulfide quantum dot of a kind of size.
Background technology
Because the size of quantum dot is less than electron wavelength, the energy of its current carrier is quantized, makes quantum dot have excellent optics, electricity and magnetic performance.Semiconductor-quantum-point because of its unique optics, electrical property in recent years because of risen people extensive concern, be widely used in the different sciemtifec and technical spheres such as bioluminescence label, biosensor, bio-imaging, bioprobe and solar cell.
II-VI family semi-conductor, especially CdS, CdSe and CdTe are also studied widely, and it can be easy to change the transmitting in visible-range by size and the preparation method of simple adjustment particle.In these materials, CdS is very important straight gap semiconductor nano material, energy gap Eg=2.42eV.CdS quantum dot can be used for the photoelectric commutator of the photoelectricity of solar cell, the light emitting diode in flat-panel monitor.Energy gap under visible-range room temperature is in 2.53 left and right.
At present, the approach of preparing of quantum dot is mainly organic phase preparation and water preparation.Quantum dot, as a kind of novel fluorescent substance, is compared with traditional organic fluorescence molecule and is had the unexistent special optical character of traditional organic fluorescence molecule.For example, the fluorescence peak width at half height of quantum dot is only 1/3rd of organic fluorescence molecule, and the intensity of fluorescence emission peak is tens times of organic fluorescence molecule.The more important thing is, the fluorescence intensity of quantum dot can not weaken under transmitting continuing for a long time, and fluorescent emission is comparatively stable, and this is that traditional organic fluorescence molecule institute is inaccessiable.Meanwhile, the novel quantum dot of preparing by organic phase, the monodispersity that particle has had, strong stability, high fluorescence quantum yield and the narrower features such as peak width at half height; But there is the features such as reagent toxicity is strong, experimental cost is high, operational danger is large.The patent No. is the presoma pyrolysis method of 200510133953.6 Chinese invention patent report, at the temperature of 140 ~ 250 ℃, carry out building-up reactions, and the reaction times reaches 4 ~ 6 hours.The hydrothermal synthesis method of the Chinese invention patent report of the patent No. 200510031067.2 carry out in autoclave and the temperature and time of building-up reactions reaches respectively 80 ~ 150 ℃ and 5 hours.The patent No. is 200810033595.5 Chinese invention patent, has synthesized at normal temperatures and pressures the controlled Cadmium Sulfide quantum of size, and synthetic multistep is carried out, and method is complicated.Therefore, find a kind of cost lower, method is simple, and the method for the synthesizing cadmium sulfide quantum dot that environmental pollution is less has realistic meaning.
Summary of the invention
Technical problem to be solved by this invention is to provide the preparation method of the controlled cadmiumsulfide quantum dot of a kind of method is simple, cost is lower, environmental pollution is little size.
For addressing the above problem, the preparation method of the cadmiumsulfide quantum dot that a kind of size of the present invention is controlled, comprises the following steps:
(1) four water cadmium nitrates and sublimed sulphur are joined in 5 ~ 15mL oleyl amine solution by 1 ~ 6 mol ratio, after mixing, obtain mixing solutions; Described mixing solutions is at room temperature stirred and is passed into rare gas element argon gas 10 ~ 15min, under the protection of rare gas element argon gas, the speed with 5 ~ 20 ℃/min is heated to 120 ~ 140 ℃ subsequently, and be incubated 15 ~ 60min at 120 ~ 140 ℃, obtain the mixing solutions of yellow transparent; The mixing solutions of described yellow transparent speed with 5 ~ 20 ℃/min under the protection of rare gas element argon gas is heated to 160 ~ 290 ℃, naturally cools to room temperature after being then incubated 20 ~ 60min at this temperature, obtains cooling solution;
(2) in described cooling solution, add 10 ~ 20mL dehydrated alcohol to have yellow mercury oxide to separate out, through ultrasonic, obtain yellow mercury oxide and reaction mother liquor after centrifugal; Described throw out washs centrifugal 3 ~ 6 times with the dehydrated alcohol of 4 ~ 10mL and the mixed solution of normal hexane, through vacuum-drying, to constant weight, obtains the yellow powder shape cadmiumsulfide quantum dot of different size size.
By following preparation method, replace above-mentioned steps (1) to prepare cooling solution: at the CdCl of 0.5 ~ 3mmol 22.5H 2in O, add 8 ~ 12mL oleyl amine solution, obtain mixed liquor A; In the sublimed sulphur of 0.5 ~ 6mmol, add 3 ~ 7mL oleyl amine solution, obtain mixed liquid B; Described mixed liquor A and described mixed liquid B are at room temperature stirred respectively and pass into rare gas element argon gas 10 ~ 15min, under the protection of rare gas element argon gas, the speed with 8 ~ 20 ℃/min is heated to 125 ~ 135 ℃ subsequently, at this temperature of this mixed liquor A, be incubated 20 ~ 40min, obtain the transparent mixing solutions of white, at this temperature of this mixed liquid B, be incubated 20 ~ 40min, obtain yellow solution; The transparent mixing solutions speed with 8 ~ 12 ℃/min under the protection of rare gas element argon gas of described white is heated to after 170 ~ 270 ℃, and described yellow solution is injected in the transparent mixing solutions of described white fast, obtains the mixing solutions of yellow transparent; The mixing solutions of this yellow transparent naturally cools to room temperature be incubated 20 ~ 40min at this temperature under the protection of rare gas element argon gas after, obtains cooling solution.
The described step (1) flow velocity of middle rare gas element argon gas is 30 ~ 60mL/min.
Described step (2) in the mixed solution of dehydrated alcohol and normal hexane the volume ratio of dehydrated alcohol and normal hexane be 2 ~ 6.
Described step (2) in ultrasonic centrifugal condition refer to that ultrasonic frequency is 50kHz ~ 56kHz, ultrasonic time is 20 ~ 60 seconds.
Described step (2) in centrifugal condition refer to that centrifugation rate is 4500 ~ 7500rpm, the time is 120 ~ 200 seconds.
Described step (2) in vacuum drying condition refer to that temperature is that 30 ~ 60 ℃, vacuum tightness are-0.07 ~-0.09MPa.
The present invention compared with prior art has the following advantages:
1, the present invention has chosen the weak inorganic cadmium of toxicity and nontoxic and oleyl amine that boiling point is higher as reaction solvent, has reduced the pollution to environment.
2, the present invention adopt that one-step synthesis (one-pot) synthesized that monodispersity is good, stability is high, fluorescence intensity is high and chemical property is good cadmiumsulfide quantum dot, not only simplified preparation technology, and reduced operation easier.
3, the present invention by four water cadmium nitrates and sublimed sulphur join contain oleyl amine solution in, carry out at a certain temperature building-up reactions.The synthetic cadmiumsulfide quantum dot of the method can pass through the size of its size of controlling reaction temperature, that is to say, the method can be controlled the glow color of the maximum absorption wavelength position of uv-vis spectra, the position of fluorescent emission wavelength and cadmiumsulfide quantum dot solution.Along with the rising of temperature of reaction, there is obvious red shift in the ultraviolet absorption peak of product as seen from Figure 2, illustrates that the particle of the higher synthetic product of temperature is larger; As can be known from Fig. 3, along with red shift has appearred in the fluorescent emission wavelength of the rising product of temperature of reaction, the higher Red Shift Phenomena of temperature is more obvious, and the size that cadmiumsulfide quantum dot is described increases with the rising of temperature of reaction.As can be seen from Figure 4, cadmiumsulfide quantum dot synthetic under differing temps can show distinct colors under ultra violet lamp, and this explanation can be synthesized the cadmiumsulfide quantum dot of different size by controlling temperature.
4, the cadmiumsulfide quantum dot of gained of the present invention is carried out to x-ray diffraction experiment, can find 2 θ=(26.465,43.943 and 52.031 .) locate to have occurred that obvious diffraction peak, these diffraction peaks correspond respectively to CdS (111), (220), (311) crystal face (referring to Fig. 1).
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in further detail.
Fig. 1 is the X ray diffracting spectrum (raw material is four water cadmium nitrates, sublimed sulphur and oleyl amine) of cadmiumsulfide quantum dot of the present invention.
Fig. 2 is ultraviolet-visible absorption spectroscopy (UV-Vis) figure of the cadmiumsulfide quantum dot under differing temps of the present invention, and wherein X-coordinate is wavelength, and ordinate zou is that (synthesis material is four water cadmium nitrates, sublimed sulphur and oleyl amine to absorbancy; Dispersion solvent is normal hexane).
Fig. 3 is photoluminescence (Photoluminescence, the PL) spectrogram of the cadmiumsulfide quantum dot under differing temps of the present invention, and wherein X-coordinate is wavelength, and ordinate zou is that (synthesis material is four water cadmium nitrates, sublimed sulphur and oleyl amine to fluorescence intensity; Dispersion solvent is normal hexane).
Fig. 4 is that (synthesis material is four water cadmium nitrates, sublimed sulphur and oleyl amine to cadmiumsulfide quantum dot solution under the differing temps of the present invention fluorescence photo under the ultraviolet lamp of 365nm wavelength; Dispersion solvent is normal hexane).
Embodiment
embodiment 1a preparation method for the cadmiumsulfide quantum dot that size is controlled, comprises the following steps:
(1) four water cadmium nitrates and sublimed sulphur are joined in 5mL oleyl amine solution by 1 mol ratio, after mixing, obtain mixing solutions.
Mixing solutions is at room temperature stirred and pass into rare gas element argon gas 10min with the flow velocity of 30mL/min; under the protection of rare gas element argon gas, the speed with 10 ℃/min is heated to 130 ℃ subsequently; and be incubated 30min at 130 ℃, obtain the mixing solutions of yellow transparent.
The mixing solutions of yellow transparent speed with 10 ℃/min under the protection of rare gas element argon gas is heated to 180 ℃, naturally cools to room temperature after being then incubated 30min at this temperature, obtains cooling solution.
(2) in cooling solution, add 15mL dehydrated alcohol to have yellow mercury oxide to separate out, after ultrasonic centrifugal 20 seconds that are 50kHz through ultrasonic frequency, obtain yellow mercury oxide and reaction mother liquor; With the dehydrated alcohol of 5mL and the mixed solution of normal hexane, the centrifugation rate with 6000rpm washs centrifugal 4 times throw out, each 120 seconds, temperature be 30 ℃, vacuum tightness for the condition of-0.07MPa under vacuum-drying to constant weight, obtain the yellow powder shape cadmiumsulfide quantum dot of different size size.
Wherein: in the mixed solution of dehydrated alcohol and normal hexane, the volume ratio of dehydrated alcohol and normal hexane (mL/mL) is 2.
embodiment 2a preparation method for the cadmiumsulfide quantum dot that size is controlled, comprises the following steps:
(1) four water cadmium nitrates and sublimed sulphur are joined in 15mL oleyl amine solution by 6 mol ratio, after mixing, obtain mixing solutions.
Mixing solutions is at room temperature stirred and pass into rare gas element argon gas 15min with the flow velocity of 60mL/min; under the protection of rare gas element argon gas, the speed with 5 ℃/min is heated to 120 ℃ subsequently; and be incubated 15min at 120 ℃, obtain the mixing solutions of yellow transparent.
The mixing solutions of yellow transparent speed with 5 ℃/min under the protection of rare gas element argon gas is heated to 160 ℃, naturally cools to room temperature after being then incubated 20min at this temperature, obtains cooling solution.
(2) in cooling solution, add 10mL dehydrated alcohol to have yellow mercury oxide to separate out, after ultrasonic centrifugal 60 seconds that are 56kHz through ultrasonic frequency, obtain yellow mercury oxide and reaction mother liquor; With the dehydrated alcohol of 4mL and the mixed solution of normal hexane, the centrifugation rate with 4500rpm washs centrifugal 3 times throw out, each 200 seconds, temperature be 60 ℃, vacuum tightness for the condition of-0.09MPa under vacuum-drying to constant weight, obtain the yellow powder shape cadmiumsulfide quantum dot of different size size.
Wherein: in the mixed solution of dehydrated alcohol and normal hexane, the volume ratio of dehydrated alcohol and normal hexane (mL/mL) is 6.
embodiment 3a preparation method for the cadmiumsulfide quantum dot that size is controlled, comprises the following steps:
(1) four water cadmium nitrates and sublimed sulphur are joined in 10mL oleyl amine solution by 3 mol ratio, after mixing, obtain mixing solutions.
Mixing solutions is at room temperature stirred and pass into rare gas element argon gas 12min with the flow velocity of 40mL/min; under the protection of rare gas element argon gas, the speed with 20 ℃/min is heated to 140 ℃ subsequently; and be incubated 60min at 140 ℃, obtain the mixing solutions of yellow transparent.
The mixing solutions of yellow transparent speed with 20 ℃/min under the protection of rare gas element argon gas is heated to 290 ℃, naturally cools to room temperature after being then incubated 60min at this temperature, obtains cooling solution.
(2) in cooling solution, add 20mL dehydrated alcohol to have yellow mercury oxide to separate out, after ultrasonic centrifugal 40 seconds that are 53kHz through ultrasonic frequency, obtain yellow mercury oxide and reaction mother liquor; With the dehydrated alcohol of 10mL and the mixed solution of normal hexane, the centrifugation rate with 7500rpm washs centrifugal 6 times throw out, each 160 seconds, temperature be 45 ℃, vacuum tightness for the condition of-0.08MPa under vacuum-drying to constant weight, obtain the yellow powder shape cadmiumsulfide quantum dot of different size size.
Wherein: in the mixed solution of dehydrated alcohol and normal hexane, the volume ratio of dehydrated alcohol and normal hexane (mL/mL) is 4.
embodiment 4a preparation method for the cadmiumsulfide quantum dot that size is controlled, comprises the following steps:
(1) at the CdCl of 1mmol 22.5H 2in O, add 8mL oleyl amine solution, obtain mixed liquor A; In the sublimed sulphur of 2mmol, add 3mL oleyl amine solution, obtain mixed liquid B.
Mixed liquor A and mixed liquid B are at room temperature stirred respectively and pass into rare gas element argon gas 10min with the flow velocity of 30mL/min; under the protection of rare gas element argon gas, the speed with 20 ℃/min is heated to 130 ℃ subsequently; this mixed liquor A is incubated 30min at 130 ℃; obtain the transparent mixing solutions of white; this mixed liquid B is incubated 30min at 130 ℃, obtains yellow solution.
The transparent mixing solutions speed with 10 ℃/min under the protection of rare gas element argon gas of white is heated to after 180 ℃, and yellow solution is injected in the transparent mixing solutions of white fast, obtains the mixing solutions of yellow transparent.The mixing solutions of this yellow transparent naturally cools to room temperature be incubated 30min at 180 ℃ under the protection of rare gas element argon gas after, obtains cooling solution.
(2) in cooling solution, add 15mL dehydrated alcohol to have yellow mercury oxide to separate out, after ultrasonic centrifugal 20 seconds that are 55kHz through ultrasonic frequency, obtain yellow mercury oxide and reaction mother liquor; With the dehydrated alcohol of 5mL and the mixed solution of normal hexane, the centrifugation rate with 4500rpm washs centrifugal 4 times throw out, each 140 seconds, temperature be 30 ℃, vacuum tightness for the condition of-0.07MPa under vacuum-drying to constant weight, obtain the yellow powder shape cadmiumsulfide quantum dot of different size size.
Wherein: in the mixed solution of dehydrated alcohol and normal hexane, the volume ratio of dehydrated alcohol and normal hexane (mL/mL) is 2.
embodiment 5a preparation method for the cadmiumsulfide quantum dot that size is controlled, comprises the following steps:
(1) at the CdCl of 0.5mmol 22.5H 2in O, add 10mL oleyl amine solution, obtain mixed liquor A; In the sublimed sulphur of 0.5mmol, add 5mL oleyl amine solution, obtain mixed liquid B.
Mixed liquor A and mixed liquid B are at room temperature stirred respectively and pass into rare gas element argon gas 15min with the flow velocity of 40mL/min; under the protection of rare gas element argon gas, the speed with 8 ℃/min is heated to 125 ℃ subsequently; this mixed liquor A is incubated 40min at 125 ℃; obtain the transparent mixing solutions of white; this mixed liquid B is incubated 40min at 125 ℃, obtains yellow solution.
The transparent mixing solutions speed with 8 ℃/min under the protection of rare gas element argon gas of white is heated to after 170 ℃, and yellow solution is injected in the transparent mixing solutions of white fast, obtains the mixing solutions of yellow transparent.The mixing solutions of this yellow transparent naturally cools to room temperature be incubated 20min at 170 ℃ under the protection of rare gas element argon gas after, obtains cooling solution.
(2) in cooling solution, add 12mL dehydrated alcohol to have yellow mercury oxide to separate out, after ultrasonic centrifugal 60 seconds that are 54kHz through ultrasonic frequency, obtain yellow mercury oxide and reaction mother liquor; With the dehydrated alcohol of 4mL and the mixed solution of normal hexane, the centrifugation rate with 7500rpm washs centrifugal 3 times throw out, each 180 seconds, temperature be 60 ℃, vacuum tightness for the condition of-0.09MPa under vacuum-drying to constant weight, obtain the yellow powder shape cadmiumsulfide quantum dot of different size size.
Wherein: in the mixed solution of dehydrated alcohol and normal hexane, the volume ratio of dehydrated alcohol and normal hexane (mL/mL) is 4.
embodiment 6a preparation method for the cadmiumsulfide quantum dot that size is controlled, comprises the following steps:
(1) at the CdCl of 3mmol 22.5H 2in O, add 12mL oleyl amine solution, obtain mixed liquor A; In the sublimed sulphur of 6mmol, add 7mL oleyl amine solution, obtain mixed liquid B.
Mixed liquor A and mixed liquid B are at room temperature stirred respectively and pass into rare gas element argon gas 12min with the flow velocity of 60mL/min; under the protection of rare gas element argon gas, the speed with 14 ℃/min is heated to 135 ℃ subsequently; this mixed liquor A is incubated 20min at 135 ℃; obtain the transparent mixing solutions of white; this mixed liquid B is incubated 20min at 135 ℃, obtains yellow solution.
The transparent mixing solutions speed with 12 ℃/min under the protection of rare gas element argon gas of white is heated to after 270 ℃, and yellow solution is injected in the transparent mixing solutions of white fast, obtains the mixing solutions of yellow transparent.The mixing solutions of this yellow transparent naturally cools to room temperature be incubated 40min at 270 ℃ under the protection of rare gas element argon gas after, obtains cooling solution.
(2) in cooling solution, add 18mL dehydrated alcohol to have yellow mercury oxide to separate out, after ultrasonic centrifugal 40 seconds that are 52kHz through ultrasonic frequency, obtain yellow mercury oxide and reaction mother liquor; With the dehydrated alcohol of 8mL and the mixed solution of normal hexane, the centrifugation rate with 6000rpm washs centrifugal 5 times throw out, each 150 seconds, temperature be 45 ℃, vacuum tightness for the condition of-0.08MPa under vacuum-drying to constant weight, obtain the yellow powder shape cadmiumsulfide quantum dot of different size size.
Wherein: in the mixed solution of dehydrated alcohol and normal hexane, the volume ratio of dehydrated alcohol and normal hexane (mL/mL) is 3.

Claims (7)

1. a preparation method for the controlled cadmiumsulfide quantum dot of size, comprises the following steps:
(1) four water cadmium nitrates and sublimed sulphur are joined in 5 ~ 15mL oleyl amine solution by 1 ~ 6 mol ratio, after mixing, obtain mixing solutions; Described mixing solutions is at room temperature stirred and is passed into rare gas element argon gas 10 ~ 15min, under the protection of rare gas element argon gas, the speed with 5 ~ 20 ℃/min is heated to 120 ~ 140 ℃ subsequently, and be incubated 15 ~ 60min at 120 ~ 140 ℃, obtain the mixing solutions of yellow transparent; The mixing solutions of described yellow transparent speed with 5 ~ 20 ℃/min under the protection of rare gas element argon gas is heated to 160 ~ 290 ℃, naturally cools to room temperature after being then incubated 20 ~ 60min at this temperature, obtains cooling solution;
(2) in described cooling solution, add 10 ~ 20mL dehydrated alcohol to have yellow mercury oxide to separate out, through ultrasonic, obtain yellow mercury oxide and reaction mother liquor after centrifugal; Described throw out washs centrifugal 3 ~ 6 times with the dehydrated alcohol of 4 ~ 10mL and the mixed solution of normal hexane, through vacuum-drying, to constant weight, obtains the yellow powder shape cadmiumsulfide quantum dot of different size size.
2. the preparation method of the controlled cadmiumsulfide quantum dot of a kind of size as claimed in claim 1, is characterized in that: by following preparation method, replace step described in claim 1 (1) to prepare cooling solution: at the CdCl of 0.5 ~ 3mmol 22.5H 2in O, add 8 ~ 12mL oleyl amine solution, obtain mixed liquor A; In the sublimed sulphur of 0.5 ~ 6mmol, add 3 ~ 7mL oleyl amine solution, obtain mixed liquid B; Described mixed liquor A and described mixed liquid B are at room temperature stirred respectively and pass into rare gas element argon gas 10 ~ 15min, under the protection of rare gas element argon gas, the speed with 8 ~ 20 ℃/min is heated to 125 ~ 135 ℃ subsequently, at this temperature of this mixed liquor A, be incubated 20 ~ 40min, obtain the transparent mixing solutions of white, at this temperature of this mixed liquid B, be incubated 20 ~ 40min, obtain yellow solution; The transparent mixing solutions speed with 8 ~ 12 ℃/min under the protection of rare gas element argon gas of described white is heated to after 170 ~ 270 ℃, and described yellow solution is injected in the transparent mixing solutions of described white fast, obtains the mixing solutions of yellow transparent; The mixing solutions of this yellow transparent naturally cools to room temperature be incubated 20 ~ 40min at this temperature under the protection of rare gas element argon gas after, obtains cooling solution.
3. the preparation method of the controlled cadmiumsulfide quantum dot of a kind of size as claimed in claim 1 or 2, is characterized in that: described step (1) in the flow velocity of rare gas element argon gas be 30 ~ 60mL/min.
4. the preparation method of the controlled cadmiumsulfide quantum dot of a kind of size as claimed in claim 1, is characterized in that: described step (2) in the mixed solution of dehydrated alcohol and normal hexane the volume ratio of dehydrated alcohol and normal hexane be 2 ~ 6.
5. the preparation method of the controlled cadmiumsulfide quantum dot of a kind of size as claimed in claim 1, is characterized in that: described step (2) in ultrasonic centrifugal condition refer to that ultrasonic frequency is 50kHz ~ 56kHz, ultrasonic time is 20 ~ 60 seconds.
6. the preparation method of the controlled cadmiumsulfide quantum dot of a kind of size as claimed in claim 1, is characterized in that: described step (2) in centrifugal condition refer to that centrifugation rate is 4500 ~ 7500rpm, the time is 120 ~ 200 seconds.
7. the preparation method of the controlled cadmiumsulfide quantum dot of a kind of size as claimed in claim 1, is characterized in that: described step (2) in vacuum drying condition refer to that temperature is that 30 ~ 60 ℃, vacuum tightness are-0.07 ~-0.09MPa.
CN201410130418.4A 2014-04-02 2014-04-02 The preparation method of the cadmiumsulfide quantum dot that a kind of size is controlled Expired - Fee Related CN103936057B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104445440A (en) * 2014-11-10 2015-03-25 西北师范大学 Preparation method of Fe1-XS nanomaterial with controllable size and shape
CN113755164A (en) * 2021-10-14 2021-12-07 汕头职业技术学院 Green and environment-friendly cadmium sulfide quantum dot preparation and manufacturing process
CN117362037A (en) * 2023-10-16 2024-01-09 潍坊卓宇新材料科技有限公司 Cadmium sulfide target piece processing technology and split processing die

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Publication number Priority date Publication date Assignee Title
CN1884093A (en) * 2006-07-03 2006-12-27 天津大学 Raw materials components for preparation sulfide of cadmium nano crystal and process for preparing same

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1884093A (en) * 2006-07-03 2006-12-27 天津大学 Raw materials components for preparation sulfide of cadmium nano crystal and process for preparing same

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104445440A (en) * 2014-11-10 2015-03-25 西北师范大学 Preparation method of Fe1-XS nanomaterial with controllable size and shape
CN104445440B (en) * 2014-11-10 2016-08-24 西北师范大学 A kind of size, the Fe of morphology controllable1-Xthe preparation method of S nano material
CN113755164A (en) * 2021-10-14 2021-12-07 汕头职业技术学院 Green and environment-friendly cadmium sulfide quantum dot preparation and manufacturing process
CN117362037A (en) * 2023-10-16 2024-01-09 潍坊卓宇新材料科技有限公司 Cadmium sulfide target piece processing technology and split processing die

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