CN105001869A - Microwave preparation method for water-soluble Ce-doped Ce:CdTe quantum dots - Google Patents
Microwave preparation method for water-soluble Ce-doped Ce:CdTe quantum dots Download PDFInfo
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- CN105001869A CN105001869A CN201510422103.1A CN201510422103A CN105001869A CN 105001869 A CN105001869 A CN 105001869A CN 201510422103 A CN201510422103 A CN 201510422103A CN 105001869 A CN105001869 A CN 105001869A
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Abstract
The invention discloses a microwave preparation method for water-soluble Ce-doped Ce:CdTe quantum dots. The method comprises the steps of adding sodium borohydride and tellurium powders in the mol ratio of 5.1:1 in water, placing the obtained product in a microwave synthesizer under the protection of nitrogen, heating at the temperature of 70-80 DEG C, stirring to react for 1-2 minutes, then heating again at the temperature of 90-95 DEG C, stirring to react for 2-3 minutes to obtain the tellurium sodium hydride solution, then adding a cadmium salt, a cerium salt and a modified water-soluble N-acetyl-L-cysteine solution in a container, injecting the above tellurium sodium hydride solution, and pumping nitrogen into the solution from top to bottom for 2-3 minutes to obtain a Ce-doped Ce:CdTe quantum dot precursor solution. The above method is energy-saving, high in efficiency, free of pollution and easy to control, wherein the heating is quick and uniform in effect.
Description
Technical field
The present invention relates to Illuminant nanometer material and biochemical analysis field, specifically, relate to a kind of microwave preparation of Ce:CdTe quantum dot of water-soluble Ce doping.
Background technology
Quantum dot is a kind of by II-VI group or iii-v is elementary composition, the inorganic semiconductor nanocrystal of diameter between 2 ~ 10nm.Because quantum dot has many superior fluorescence properties, make it obtain at biochemical analysis and biomedical sector and apply quite widely.Meanwhile, the synthesis of high quality, Multifunction fluorescent quantum dot also arouses great concern gradually.
At present, people mainly use conventional hydrothermal method to synthesize quantum dot, but the usual quantum yield of quantum dot of conventional hydrothermal method synthesis is lower, and the quantum dot required time that red fluorescence is launched in synthesis is longer, and peak width at half height is wider.The conventional hydrothermal method synthesis particle size growth speed of quantum dot and the poor major cause of crystal property are conventional hydrothermal methods is a kind of slowly heat-processed, dependence thermal conduction, thermal convection realize, heating feature is from sample surfaces, heat energy ecto-entad is propagated, and causes sample to be heated uneven.And research uses microwave method to prepare small particle size, during the uniform nanoparticle of form, microwave method has the incomparable superiority of other method.
Summary of the invention
An object of the present invention is to solve at least the problems referred to above and/or defect, and the advantage will illustrated at least is below provided.
A further object of the invention is just to provide a kind of microwave preparation of Ce:CdTe quantum dot of water-soluble Ce doping.
In order to realize according to these objects of the present invention and other advantages, provide a kind of microwave preparation of Ce:CdTe quantum dot of water-soluble Ce doping.It is as follows that the method comprising the steps of:
Step one, by mol ratio be 5.1: 1 sodium borohydride and tellurium powder be placed in water; Under nitrogen protection, this aqueous solution of sodium borohydride and tellurium powder is placed in Microwave synthesize instrument, is heated to 70 ~ 80 DEG C of stirring reaction 1-2 minute, be then heated to 90-95 DEG C of stirring reaction 2-3 minute, obtain sodium hydrogen telluride solution;
Step 2, add the water-soluble N-acetyl-L-cysteine solution of cadmium salt, cerium salt and modifier in a reservoir, wherein Cd
2+concentration be 0.12mol/L, Cd
2+: Ce
2+mol ratio be 1: 0.2, the pH value of regulator solution is 13.1, under nitrogen protection, be in the sodium hydrogen telluride solution prepared of this solution-injecting step one of 13.1 by pH value, be that the ullage of this solution of 13.1 passes into nitrogen 2-3 minute below liquid level again from pH value, obtain the Ce:CdTe quantum dot precursor solution of Ce doping;
Step 3, the Ce:CdTe quantum dot precursor solution that Ce adulterates is placed in microwave reactor, under power 100W, is heated to 100-120 DEG C of reaction 5-10 second, obtains the Ce:CdTe quantum dot solution that water-soluble Ce adulterates;
Wherein, in step one and step 2, Cd in reactant
2+: Ce
2+: the mol ratio of N-acetyl-L-cysteine: NaHTe is 1: 0.2: 3.6: 0.09.
Preferably, the mass parts of the water of step one is 6-20 part.
Preferably, cadmium salt is Cadmium chloride fine powder, and described cerium salt is cerous sulfate.
Preferably, tellurium powder content is 99.9%, and the specification of described tellurium powder is 120-150 mesh sieve.
Preferably, in step 3, the Ce:CdTe quantum dot precursor solution that Ce adulterates being placed in the type of heating of microwave reactor, can be after being first heated to 100 DEG C of reaction 1-2 seconds, is converted to 120 DEG C of reaction 5-6 seconds.
Preferably, also comprise step 4, the Ce:CdTe quantum dot solution sealing of being adulterated by water-soluble Ce is placed in microwave reactor and is heated to 75-85 DEG C, keep taking out for 2-3 minute.
Beneficial effect of the present invention: the present invention adopts the mode of microwave radiation to heat, makes heat-up rate in reaction process fast, easy to operate, the generation of Reaction time shorten and minimizing byproduct, and cost is low, simple to operate, is suitable for suitability for industrialized production.The present invention utilizes the penetrativity of microwave comparatively strong, and can be radiated by the inside of heated sample, first raised temperature from sample center, heat energy is propagated from inside to outside, and system of being heated homogeneous temperature makes obviously to accelerate the reaction times, improves heating efficiency.Thus possess its more particular advantages have (1) microwave method to be the body heating that material causes because of the loss of self medium, can realize the stirring on molecular level, heat-up rate is fast, homogeneous heating; (2) because the dielectric characteristics of material of the present invention self determines the ability that it absorbs microwave, therefore microwave method can carry out selectivity heating to each component in inventive mixture material; (3) the microwave method heating induction phase is extremely short, does not even almost have inductive phase, and then effectively prevent the generation of other crystalline phase; (4) microwave method is without lag-effect, overcomes conventional hydrothermal container and heats unequal shortcoming, safety non-pollution, energy-efficient.
Accompanying drawing explanation
Fig. 1 is the fluorescence spectrum figure of the Ce:CdTe quantum dot of the Ce doping that the present invention prepares.
Embodiment
Following examples further illustrate of the present invention, but absolutely not limit the scope of the present invention.Elaborate the present invention further referring to embodiment, but it will be appreciated by those skilled in the art that the present invention is not limited to the preparation method of these embodiments and use.
Embodiment 1
A kind of microwave preparation of Ce:CdTe quantum dot of water-soluble Ce doping comprises the following steps:
Step one, by mol ratio be 5.1: 1 sodium borohydride and content be 99.9% tellurium powder be placed in water, the consumption of water is 10 parts of mass parts, and under nitrogen protection, be placed in Microwave synthesize instrument, be heated to 75 DEG C of stirring reactions 1 minute, then be heated to 92 DEG C of stirring reactions 3 minutes, obtain sodium hydrogen telluride solution; Wherein, tellurium powder specification is 120 mesh sieves;
Step 2, add the water-soluble N-acetyl-L-cysteine solution of Cadmium chloride fine powder, cerous sulfate and modifier in a reservoir, wherein Cd
2+concentration be 0.12mol/L, Cd
2+: Ce
2+mol ratio be 1: 0.2, the pH value of regulator solution is 13.1, under nitrogen protection, in implantation step one preparation sodium hydrogen telluride solution, then above solution toward below pass into nitrogen 3 minutes, obtain Ce doping Ce:CdTe quantum dot precursor solution;
Step 3, by Ce adulterate Ce:CdTe quantum dot precursor solution be placed in microwave reactor, be first heated under power 100W 100 DEG C reaction 2 seconds after, be converted to 120 DEG C reaction 5 seconds, obtain water-soluble Ce adulterate Ce:CdTe quantum dot solution;
Step 4, the Ce:CdTe quantum dot solution sealing of being adulterated by water-soluble Ce are placed in microwave reactor and are heated to 80 DEG C, keep taking out for 3 minutes;
Wherein, in step one and step 2, Cd in reactant
2+: Ce
2+: the mol ratio of N-acetyl-L-cysteine: NaHTe is 1: 0.2: 3.6: 0.09.
Embodiment 2
A kind of microwave preparation of Ce:CdTe quantum dot of water-soluble Ce doping comprises the following steps:
Step one, by mol ratio be 5.1: 1 sodium borohydride and content be 99.9% tellurium powder be placed in water, the consumption of water is 20 parts of mass parts, under nitrogen protection, be placed in Microwave synthesize instrument, be heated to 70 DEG C of stirring reactions 2 minutes, then be heated to 90 DEG C of stirring reactions 3 minutes, obtain sodium hydrogen telluride solution; Wherein, tellurium powder specification is 120 mesh sieves;
Step 2, add the water-soluble N-acetyl-L-cysteine solution of Cadmium chloride fine powder, cerous sulfate and modifier in a reservoir, wherein Cd
2+concentration be 0.12mol/L, Cd
2+: Ce
2+mol ratio be 1: 0.2, the pH value of regulator solution is 13.1, under nitrogen protection, in implantation step one preparation sodium hydrogen telluride solution, then above solution toward below pass into nitrogen 2 minutes, obtain Ce doping Ce:CdTe quantum dot precursor solution;
Step 3, the Ce:CdTe quantum dot precursor solution that Ce adulterates is placed in microwave reactor, under power 100W, is heated to 100 DEG C of reaction 5-10 seconds, obtains the Ce:CdTe quantum dot solution that water-soluble Ce adulterates;
Wherein, in step one and step 2, Cd in reactant
2+: Ce
2+: the mol ratio of N-acetyl-L-cysteine: NaHTe is 1: 0.2: 3.6: 0.09.
Embodiment 3
A kind of microwave preparation of Ce:CdTe quantum dot of water-soluble Ce doping comprises the following steps:
Step one, 0.2067gTe powder and 0.3125g NaBH4 are put in container, add 5mL distilled water, under nitrogen protection, be placed in Microwave synthesize instrument, at heating 70 DEG C, stirring reaction 2 minutes, is then heated to 95 DEG C of stirring reactions 3 minutes, obtains sodium hydrogen telluride NaHTe solution; Wherein, tellurium powder specification is 150 mesh sieves;
Step 2, by 0.8221g CdCl
2, 0.2910g Ce (SO
4)
2be dissolved in 30mL distilled water with 2.1149gN-acetyl-Cys, wherein Cd
2+concentration be 0.12mol/L, Cd
2+: Ce
2+mol ratio be 1: 0.2, the pH value of regulator solution is 13.1, under nitrogen protection, in implantation step one preparation sodium hydrogen telluride NaHTe solution, then above solution toward below pass into nitrogen 2 minutes, obtain Ce doping Ce:CdTe quantum dot precursor solution;
Step 3, by Ce adulterate Ce:CdTe quantum dot precursor solution be placed in microwave reactor, be heated under power 100W 100 DEG C reaction 5 seconds, obtain water-soluble Ce adulterate Ce:CdTe quantum dot solution;
Wherein, in step one and step 2, Cd in reactant
2+: Ce
2+: the mol ratio of N-acetyl-L-cysteine: NaHTe is 1: 0.2: 3.6: 0.09.
Above-mentioned reaction modifier used is that stability is high, the N-acetyl-L-cysteine of environmental friendliness, good biocompatibility.
Embodiment 4
A kind of microwave preparation of Ce:CdTe quantum dot of water-soluble Ce doping comprises the following steps:
Step one, by mol ratio be 5.1: 1 sodium borohydride and content be 99.9% tellurium powder be placed in water, the consumption of water is 6 parts of mass parts, under nitrogen protection, be placed in Microwave synthesize instrument, be heated to 80 DEG C of stirring reactions 1 minute, then be heated to 95 DEG C of stirring reactions 2 minutes, obtain sodium hydrogen telluride solution; Wherein, tellurium powder specification is 140 mesh sieves;
Step 2, add the water-soluble N-acetyl-L-cysteine solution of Cadmium chloride fine powder, cerous sulfate and modifier in a reservoir, wherein Cd
2+concentration be 0.12mol/L, Cd
2+: Ce
2+mol ratio be 1: 0.2, the pH value of regulator solution is 13.1, under nitrogen protection, in implantation step one preparation sodium hydrogen telluride solution, then above solution toward below pass into nitrogen 3 minutes, obtain Ce doping Ce:CdTe quantum dot precursor solution;
Step 3, by Ce adulterate Ce:CdTe quantum dot precursor solution be placed in microwave reactor, be heated under power 100W 120 DEG C reaction 10 seconds, obtain water-soluble Ce adulterate Ce:CdTe quantum dot solution;
Wherein, in step one and step 2, Cd in reactant
2+: Ce
2+: the mol ratio of N-acetyl-L-cysteine: NaHTe is 1: 0.2: 3.6: 0.09.
The Ce:CdTe quantum dot productive rate of the water-soluble Ce doping of above-described embodiment gained is high, fluorescence property is excellent, good water solubility, fluorescence emission wavelengths is adjustable, good biocompatibility, toxicity are low, can be used as novel fluorescence nano-probe, is widely used in biochemical analysis and biomedical sector.Shown in Figure 1, the fluorescence emission wavelengths of the Ce:CdTe quantum dot solution of the water-soluble Ce doping that the present embodiment obtains is adjustable, and variable range reaches 500-650nm.
Although embodiment of the present invention are open as above, but it is not restricted to listed in specification sheets and embodiment utilization, it can be applied to various applicable the field of the invention completely, for those skilled in the art, can easily realize other amendment, therefore do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details and shown here embodiment.
Claims (6)
1. a microwave preparation for the Ce:CdTe quantum dot of water-soluble Ce doping, is characterized in that, comprise the following steps:
Step one, by mol ratio be 5.1: 1 sodium borohydride and tellurium powder be placed in water; Under nitrogen protection, this aqueous solution of sodium borohydride and tellurium powder is placed in Microwave synthesize instrument, is heated to 70 ~ 80 DEG C of stirring reaction 1-2 minute, be then heated to 90-95 DEG C of stirring reaction 2-3 minute, obtain sodium hydrogen telluride solution;
Step 2, add the water-soluble N-acetyl-L-cysteine solution of cadmium salt, cerium salt and modifier in a reservoir, wherein Cd
2+concentration be 0.12mol/L, Cd
2+: Ce
2+mol ratio be 1: 0.2, the pH value of regulator solution is 13.1, under nitrogen protection, be in the sodium hydrogen telluride solution prepared of this solution-injecting step one of 13.1 by pH value, be that the ullage of this solution of 13.1 passes into nitrogen 2-3 minute below liquid level again from pH value, obtain the Ce:CdTe quantum dot precursor solution of Ce doping;
Step 3, the Ce:CdTe quantum dot precursor solution that Ce adulterates is placed in microwave reactor, under power 100W, is heated to 100-120 DEG C of reaction 5-10 second, obtains the Ce:CdTe quantum dot solution that water-soluble Ce adulterates;
Wherein, in step one and step 2, Cd in reactant
2+: Ce
2+: the mol ratio of N-acetyl-L-cysteine: NaHTe is 1: 0.2: 3.6: 0.09.
2. the microwave preparation of the Ce:CdTe quantum dot of water-soluble Ce doping according to claim 1, it is characterized in that, the mass parts of the water of described step one is 6-20 part.
3. the microwave preparation of the Ce:CdTe quantum dot of water-soluble Ce doping according to claim 1, it is characterized in that, described cadmium salt is Cadmium chloride fine powder, and described cerium salt is cerous sulfate.
4. the microwave preparation of the Ce:CdTe quantum dot of water-soluble Ce doping according to claim 1, it is characterized in that, described tellurium powder content is 99.9%, and the specification of described tellurium powder is 120-150 mesh sieve.
5. according to the microwave preparation of the Ce:CdTe quantum dot of the water-soluble Ce doping described in any one of claim 1-4, it is characterized in that, in described step 3, the Ce:CdTe quantum dot precursor solution that Ce adulterates is placed in microwave reactor, after being heated to 100 DEG C of reaction 1-2 seconds, be converted to 120 DEG C of reaction 5-6 seconds.
6. the microwave preparation of the Ce:CdTe quantum dot of water-soluble Ce doping according to claim 5, it is characterized in that, also comprise step 4, the Ce:CdTe quantum dot solution sealing of being adulterated by water-soluble Ce is placed in microwave reactor and is heated to 75-85 DEG C, keep taking out for 2-3 minute.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115924861A (en) * | 2021-12-13 | 2023-04-07 | 中科合肥智慧农业协同创新研究院 | Nano sensing system based on Ce-CdTe QDs fluorescence and application thereof in levofloxacin detection |
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Cited By (2)
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| CN115924861A (en) * | 2021-12-13 | 2023-04-07 | 中科合肥智慧农业协同创新研究院 | Nano sensing system based on Ce-CdTe QDs fluorescence and application thereof in levofloxacin detection |
| CN115924861B (en) * | 2021-12-13 | 2024-05-10 | 中科合肥智慧农业协同创新研究院 | Ce-CdTe QDs fluorescence-based nano sensing system and application thereof in levofloxacin detection |
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