CN104495764B - A kind of cadmium telluride quantum dot and preparation method thereof - Google Patents
A kind of cadmium telluride quantum dot and preparation method thereof Download PDFInfo
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Abstract
The present invention provides the preparation method of a kind of cadmium telluride quantum dot, comprises the following steps: A) sodium bisulphite formaldehyde, tellurium simple substance and water are mixed in the basic conditions, react, obtain tellurium precursor；B) in oxygen-free environment, by cadmium source, TGA and described step A) the tellurium precursor that obtains mixes, reacts, obtain cadmium telluride quantum dot.The preparation method of the cadmium telluride quantum dot that the present invention provides is with sodium bisulphite formaldehyde as reducing agent, reaction condition is gentleer, it is easier to control, and, sodium bisulphite formaldehyde is cheap and easily-available, and cost is relatively low, and the cadmium telluride quantum dot fluorescence quantum yield obtained is higher, test result indicate that, the fluorescence quantum yield of the cadmium telluride quantum dot that the preparation method provided according to the present invention obtains can reach 65～70%.Present invention also offers a kind of cadmium telluride quantum dot.
Description
Technical field
The invention belongs to field of inorganic materials, particularly relate to a kind of cadmium telluride quantum dot and preparation method thereof.
Background technology
Quantum dot, can be described as again nanocrystalline, is a kind of nano-particle elementary composition by II-VI group or iii-v.Quantum
The particle diameter of point is typically in the range of between 1～10nm, and owing to electronics and hole are by quantum confinement, continuous print band structure becomes and has point
The discrete energy levels structure of sub-feature, can launch fluorescence after being excited.Based on quantum effect, quantum dot is at solaode, luminous
Device, the field such as optical bio labelling is with a wide range of applications.Scientist has invented many different methods and has manufactured
Quantum dot, and expect that this nano material has in the nanoelectronics (nanoelectronics) of 21st century greatly
Application potential.
Cadmium telluride quantum dot is applied to numerous areas because of the optics and electronics character of its uniqueness, such as bio-sensing, biology
Imaging and luminescent device etc..In order to improve the luminosity of quantum dot, develop various synthetic method, including organic side
Method, aqueous phase method etc., for synthesizing high-quality quantum dot in organic facies, widely used high-temperature hot injecting method generally needs
To carry out being rapidly injected of presoma at very high temperatures, it is also desirable at high temperature realize the growth of quantum dot, and nucleation
Speed and the quality of product affected relatively big by predecessor injection rate and stirring intensity, and the amount of preparation is very limited.This
A little factors all limit the popularization in prepared by quantum dot scale of the high-temperature hot injection.
Compared to organic procedures, aqueous phase method being rapidly injected without precursor solution, the quantum dot of synthesis is more friendly,
Simple to operate, low for equipment requirements, thus be suitable for commercially producing on a large scale.And there is more wide application prospect.
In existing aqueous synthesis method, the preparation method of negative bivalence tellurium ion mainly use sodium borohydride reduction tellurium powder,
The tellurium such as tellurium dioxide or Sodium tellurite. source obtains sodium hydrogen telluride, but, this reaction the soonest, too violent, react wayward.
Summary of the invention
The invention provides a kind of cadmium telluride quantum dot and preparation method thereof, the system of the cadmium telluride quantum dot that the present invention provides
Preparation Method, on the premise of maintaining higher fluorescence quantum yield, reacts gentleer, is easily controlled.
The present invention provides the preparation method of a kind of cadmium telluride quantum dot, comprises the following steps:
A) sodium bisulphite formaldehyde, tellurium simple substance and water are mixed in the basic conditions, react, obtain tellurium precursor；
B) in oxygen-free environment, by cadmium source, TGA and described step A) the tellurium precursor that obtains mixes, reacts,
Obtain cadmium telluride quantum dot.
Preferably, described sodium bisulphite formaldehyde is (10～20) with the mol ratio of tellurium simple substance: 1.
Preferably, described step A) in reaction under reflux conditions carry out；
Described step A) in reaction temperature be 90～110 DEG C；
Described step A) in reaction time be 20～60min.
Preferably, described step B) specifically include following steps:
Cadmium source, TGA and alkaline medium are mixed, obtains cadmium precursor；
In oxygen-free environment, described cadmium precursor is mixed with described tellurium precursor, reacts, obtain cadmium telluride quantum dot.
Preferably, the pH value of described cadmium precursor is 11～12.
Preferably, the mol ratio of described cadmium source and described TGA is 1:(0.5～5).
Preferably, the mol ratio in described tellurium simple substance and cadmium source is 0.5:(0.25～3).
Preferably, described cadmium source includes one or more in Caddy (Cleary), cadmium nitrate, cadmium sulfate and cadmium perchlorate；
Described alkaline medium includes sodium hydroxide and/or potassium hydroxide.
Preferably, described step B) in reaction under reflux conditions carry out；
Described step B) in reaction temperature be 90～110 DEG C；
Described step B) in reaction time be 5～750min.
The present invention provides a kind of cadmium telluride quantum dot, makes according to the preparation method described in technique scheme, described tellurium
The particle diameter of cadmium quantum dot is 0.5～10nm；
The fluorescence emission wavelengths of described cadmium telluride quantum dot is 532～670nm.
The present invention provides the preparation method of a kind of cadmium telluride quantum dot, comprises the following steps: A) by sodium bisulphite formaldehyde,
Tellurium simple substance and water mix in the basic conditions, react, and obtain tellurium precursor；B) in oxygen-free environment, by cadmium source, TGA
With described step A) the tellurium precursor that obtains mixes, reacts, obtain cadmium telluride quantum dot.The cadmium telluride quantum that the present invention provides
The preparation method of point is with sodium bisulphite formaldehyde as reducing agent, and reaction condition is gentleer, it is easier to control, and, sulphoxylic acid
Hydrogen sodium formaldehyde is cheap and easily-available, and cost is relatively low, and the cadmium telluride quantum dot fluorescence quantum yield obtained is higher, test result indicate that,
The fluorescence quantum yield of the cadmium telluride quantum dot that the preparation method provided according to the present invention obtains can reach 65～70%.
Accompanying drawing explanation
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
In having technology to describe, the required accompanying drawing used is briefly described, it should be apparent that, the accompanying drawing in describing below is only this
Inventive embodiment, for those of ordinary skill in the art, on the premise of not paying creative work, it is also possible to according to
The accompanying drawing provided obtains other accompanying drawing.
Fig. 1 is the fluorescence spectrum figure of the cadmium telluride quantum dot that the embodiment of the present invention 1～8 obtains；
The fluorescence quantum yield of the cadmium telluride quantum dot that Fig. 2 is the embodiment of the present invention 1 and embodiment 9～11 obtains；
The fluorescence quantum yield of the cadmium telluride quantum dot that Fig. 3 is the embodiment of the present invention 1 and embodiment 12～15 obtains；
The abosrption spectrogram of the cadmium telluride quantum dot that Fig. 4 is the embodiment of the present invention 1 and embodiment 16～24 obtains；
Fig. 5 is the fluorescence spectrum figure of the cadmium telluride quantum dot that the embodiment of the present invention 17,22 and 24 obtains.
Detailed description of the invention
The invention provides the preparation method of a kind of cadmium telluride quantum dot, comprise the following steps:
A) sodium bisulphite formaldehyde, tellurium simple substance and water are mixed in the basic conditions, react, obtain tellurium precursor；
B) in oxygen-free environment, by cadmium source, TGA and described step A) the tellurium precursor that obtains mixes, reacts,
Obtain cadmium telluride quantum dot.
The preparation method reaction gentleness of the cadmium telluride quantum dot that the present invention provides, low cost, and the cadmium telluride amount obtained
The fluorescence quantum yield of son point is higher.
Sodium bisulphite formaldehyde, tellurium simple substance and water are mixed by the present invention in the basic conditions, react, before obtaining tellurium
Body.Described tellurium simple substance, sodium hydroxide and sodium bisulphite formaldehyde are preferably added to the water by the present invention, react, obtain telluride
Sodium, more preferably adds described tellurium simple substance, sodium hydroxide and sodium bisulphite formaldehyde in the water being stirred vigorously, reacts,
Obtain telluride sodium.In the present invention, described tellurium simple substance is preferably tellurium powder, and described sodium bisulphite formaldehyde is commonly called as rongalite, price
Cheap and be readily obtained, make reaction gentle in the preparation process of telluride sodium quantum dot, be easily controlled.In the embodiment of the present invention
In, described sodium bisulphite formaldehyde is preferably (10～20) with the mol ratio of tellurium simple substance: 1, more preferably (12～18): 1, optimum
Elect 16:1 as；The present invention does not has special restriction to the consumption of described sodium hydroxide and water, it is possible to make the pH value of above-mentioned reaction exist
Between 10～12.
During the present invention obtains tellurium precursor, the time of described reaction be preferably 20～60min, more preferably 25～
55min, most preferably 30～50min；The temperature of described reaction is preferably 90～110 DEG C, more preferably 95～105 DEG C, optimum
Elect 100 DEG C as.The present invention the most under reflux conditions carries out described reaction, and present invention preferably employs connection has the three of condensing unit
Mouth flask carries out above-mentioned back flow reaction, and before described back flow reaction starts, experimental provision used is preferably led to nitrogen by the present invention
20min, with the oxygen in removal device.
After obtaining tellurium precursor, in the absence of oxygen, the present invention is by cadmium source, TGA and described step A) tellurium that obtains
Precursor mixes, and reacts, obtains cadmium telluride quantum dot.Cadmium source, TGA and alkaline medium are preferably mixed by the present invention,
To cadmium precursor；In oxygen-free environment, described cadmium precursor is mixed with described tellurium precursor, reacts, obtain cadmium telluride quantum dot.
In the present invention, described cadmium source preferably includes one or more in Caddy (Cleary), cadmium nitrate, cadmium sulfate and cadmium perchlorate, more excellent
Elect Caddy (Cleary) and/or cadmium nitrate as；Described alkaline medium preferably includes sodium hydroxide and/or potassium hydroxide, more preferably hydrogen-oxygen
Change sodium；Described cadmium source is preferably 1:(0.5～5 with the mol ratio of TGA), more preferably 1:(1～4.5), most preferably 1:
(1.5～4)；The mol ratio in described tellurium simple substance and described cadmium source is preferably 0.5:(0.25～3), more preferably 0.5:(0.5～
2.5).The present invention does not has special restriction to the consumption of described alkaline medium, it is possible to by the pH regulator of described cadmium precursor to 11～
12, preferably the pH value of described cadmium precursor is regulated to 11.6.The present invention preferably carries out described preparing cadmium in glass funnel
The reaction of precursor, in order to be connected with the there-necked flask used in technique scheme.
After obtaining described cadmium precursor, described cadmium precursor is preferably mixed by the present invention with water, obtains cadmium precursor solution, adds water to
The cumulative volume of described cadmium precursor solution is 2mL.
After obtaining cadmium precursor, in oxygen-free environment, the present invention will state cadmium precursor and mix with described tellurium precursor, react,
Obtain cadmium telluride quantum dot.In the present invention, the time of described reaction is preferably 5～750min, more preferably 10～740min,
Most preferably 20～730min；The temperature of described reaction is preferably 90～110 DEG C, more preferably 95～105 DEG C, most preferably
100℃.The present invention the most under reflux conditions carries out described reaction, concrete, and preferably to prepare cadmium precursor anti-by above-mentioned for the present invention
The glass funnel answered is connected on the there-necked flask used by described tellurium precursor, after prepared by cadmium precursor, is led to by described device
Nitrogen 5min, the oxygen in removing device, then the cadmium precursor in described glass funnel is added rapidly in there-necked flask
In tellurium precursor, at 100 DEG C, carry out back flow reaction, obtain cadmium telluride quantum dot.
Present invention also offers a kind of cadmium telluride quantum dot, make according to the preparation method described in technique scheme,
In the present invention, the particle diameter of described cadmium telluride quantum dot is 0.5～10nm, preferably 1～9nm, more preferably 2～8nm；Described tellurium
The fluorescence emission wavelengths of cadmium quantum dot is 532～670nm, preferably 550～650nm.
The present invention is according to the fluorescence quantum yield of the calculated cadmium telluride quantum dot of formula shown in formula 1, in formula 1, QYQD
And QYRG6It is testing sample and the quantum yield of standard dyes Rhodamine G 6 respectively；mQDAnd mRG6It is testing sample and standard respectively
The measurement slope of dye, rhodamine G6；η represents refractive index, η=1.361 of ethanol, η=1.333 of water.Result of calculation shows,
The fluorescence quantum yield of the cadmium telluride quantum dot that the present invention obtains is between 65～70%.
The present invention provides the preparation method of a kind of cadmium telluride quantum dot, comprises the following steps: A) by sodium bisulphite formaldehyde,
Tellurium simple substance and water mix in the basic conditions, react, and obtain tellurium precursor；B) in oxygen-free environment, by cadmium source, TGA
With described step A) the tellurium precursor that obtains mixes, reacts, obtain cadmium telluride quantum dot.The cadmium telluride quantum that the present invention provides
The preparation method of point is with sodium bisulphite formaldehyde as reducing agent, and reaction condition is gentleer, it is easier to control, and, sulphoxylic acid
Hydrogen sodium formaldehyde is cheap and easily-available, and cost is relatively low, and the cadmium telluride quantum dot fluorescence quantum yield obtained is higher, test result indicate that,
The fluorescence quantum yield of the cadmium telluride quantum dot that the preparation method provided according to the present invention obtains can reach 65～70%.
In order to further illustrate the present invention, a kind of cadmium telluride quantum dot of the present invention being provided below in conjunction with embodiment and
Preparation method is described in detail, but can not be understood as limiting the scope of the present invention.
In the examples below, the excitation wavelength lambda of fluorescence spectrum detectionex=394nm.
Embodiment 1
By there-necked flask nitrogen deoxygenation 20 minutes, in there-necked flask, then add 3mL water, be stirred, then depend on
Secondary toward addition 0.0013g tellurium powder, 0.02g sodium hydroxide and 0.025g sodium bisulphite formaldehyde in the water being stirred vigorously, then
There-necked flask is connected condensing unit, refluxes 40 minutes under the conditions of 100 DEG C, obtain tellurium precursor solution.
Caddy (Cleary) and the TGA that 30 μ L concentration are 1mol/L that 200 μ L concentration are 100mmol/L are joined and three
In the glass funnel that mouth flask and condensing unit connect, with sodium hydrate regulator solution pH to 11.6, add water to solution the most afterwards
Cumulative volume is 2mL, obtains cadmium precursor solution.
Device is led to nitrogen deoxygenation 5min, then the cadmium precursor solution in glass funnel is rapidly joined in nitrogen environment
In tellurium precursor solution in there-necked flask, under the conditions of 100 DEG C, reflux condensation mode naturally cooled to room temperature after 30 minutes, obtained tellurium
Cadmium quantum dot.
The cadmium telluride quantum dot that the present embodiment is obtained by the present invention has carried out fluorescence spectrum detection, and result is as it is shown in figure 1, scheme
The fluorescence spectrum figure of 1 cadmium telluride quantum dot obtained for the embodiment of the present invention 1～8.
The present invention calculates the fluorescence quantum yield of the cadmium telluride quantum dot that the present embodiment obtains according to technique scheme
(PLQY), result is as in figure 2 it is shown, the fluorescence of Fig. 2 is the embodiment of the present invention 1 and embodiment 9～11 obtains cadmium telluride quantum dot
Quantum yield.In Fig. 2,2 is the fluorescence quantum yield of the cadmium telluride quantum dot that the embodiment of the present invention 1 obtains.As shown in Figure 2, originally
The fluorescence quantum yield of the cadmium telluride quantum dot that embodiment obtains is 66%.
Embodiment 2
Preparing cadmium telluride quantum dot according to the technical scheme in embodiment 1, except for the difference that, the present embodiment uses 16 μ L
Concentration is that the TGA of 1mol/L replaces the 30 μ L concentration used in embodiment 1 to be the TGA of 1mol/L.
The cadmium telluride quantum dot that the present embodiment is obtained by the present invention has carried out fluorescence spectrum detection, and result is as it is shown in figure 1, scheme
The fluorescence spectrum figure of 1 cadmium telluride quantum dot obtained for the embodiment of the present invention 1～8.
Embodiment 3
Preparing cadmium telluride quantum dot according to the technical scheme in embodiment 1, except for the difference that, the present embodiment uses 20 μ L
Concentration is that the TGA of 1mol/L replaces the 30 μ L concentration used in embodiment 1 to be the TGA of 1mol/L.
The cadmium telluride quantum dot that the present embodiment is obtained by the present invention has carried out fluorescence spectrum detection, and result is as it is shown in figure 1, scheme
The fluorescence spectrum figure of 1 cadmium telluride quantum dot obtained for the embodiment of the present invention 1～8.
Embodiment 4
Preparing cadmium telluride quantum dot according to the technical scheme in embodiment 1, except for the difference that, the present embodiment uses 40 μ L
Concentration is that the TGA of 1mol/L replaces the 30 μ L concentration used in embodiment 1 to be the TGA of 1mol/L.
The cadmium telluride quantum dot that the present embodiment is obtained by the present invention has carried out fluorescence spectrum detection, and result is as it is shown in figure 1, scheme
The fluorescence spectrum figure of 1 cadmium telluride quantum dot obtained for the embodiment of the present invention 1～8.
Embodiment 5
Preparing cadmium telluride quantum dot according to the technical scheme in embodiment 1, except for the difference that, the present embodiment uses 50 μ L
Concentration is that the TGA of 1mol/L replaces the 30 μ L concentration used in embodiment 1 to be the TGA of 1mol/L.
The cadmium telluride quantum dot that the present embodiment is obtained by the present invention has carried out fluorescence spectrum detection, and result is as it is shown in figure 1, scheme
The fluorescence spectrum figure of 1 cadmium telluride quantum dot obtained for the embodiment of the present invention 1～8.
Embodiment 6
Preparing cadmium telluride quantum dot according to the technical scheme in embodiment 1, except for the difference that, the present embodiment uses 60 μ L
Concentration is that the TGA of 1mol/L replaces the 30 μ L concentration used in embodiment 1 to be the TGA of 1mol/L.
The cadmium telluride quantum dot that the present embodiment is obtained by the present invention has carried out fluorescence spectrum detection, and result is as it is shown in figure 1, scheme
The fluorescence spectrum figure of 1 cadmium telluride quantum dot obtained for the embodiment of the present invention 1～8.
Embodiment 7
Preparing cadmium telluride quantum dot according to the technical scheme in embodiment 1, except for the difference that, the present embodiment uses 80 μ L
Concentration is that the TGA of 1mol/L replaces the 30 μ L concentration used in embodiment 1 to be the TGA of 1mol/L.
The cadmium telluride quantum dot that the present embodiment is obtained by the present invention has carried out fluorescence spectrum detection, and result is as it is shown in figure 1, scheme
The fluorescence spectrum figure of 1 cadmium telluride quantum dot obtained for the embodiment of the present invention 1～8.
Embodiment 8
Preparing cadmium telluride quantum dot according to the technical scheme in embodiment 1, except for the difference that, the present embodiment uses 100 μ
L concentration is that the TGA of 1mol/L replaces the 30 μ L concentration used in embodiment 1 to be the TGA of 1mol/L.
The cadmium telluride quantum dot that the present embodiment is obtained by the present invention has carried out fluorescence spectrum detection, and result is as it is shown in figure 1, scheme
The fluorescence spectrum figure of 1 cadmium telluride quantum dot obtained for the embodiment of the present invention 1～8.In Fig. 1, curve 1 is the embodiment of the present invention 2
The fluorescent spectrum curve of the cadmium telluride quantum dot obtained；Curve 2 is the fluorescence of the cadmium telluride quantum dot that the embodiment of the present invention 3 obtains
The curve of spectrum；Curve 3 is the fluorescent spectrum curve of the cadmium telluride quantum dot that the embodiment of the present invention 1 obtains；Curve 4 is that the present invention is real
Execute the fluorescent spectrum curve of the cadmium telluride quantum dot that example 4 obtains；Curve 5 is the cadmium telluride quantum dot that the embodiment of the present invention 5 obtains
Fluorescent spectrum curve；Curve 6 is the fluorescent spectrum curve of the cadmium telluride quantum dot that the embodiment of the present invention 6 obtains；Curve 7 is this
The fluorescent spectrum curve of the cadmium telluride quantum dot that inventive embodiments 7 obtains；Curve 8 is the cadmium telluride that the embodiment of the present invention 8 obtains
The fluorescent spectrum curve of quantum dot.As seen from Figure 1, the amount of stabilizer TGA (TGA) telluride to synthesis TGA protection
The photoluminescent property of cadmium quantum dot has material impact, and the amount of stabilizer T GA increases, and the wavelength of fluorescence of synthesis quantum dot is elongated.
Embodiment 9
Preparing cadmium telluride quantum dot according to the technical scheme in embodiment 1, except for the difference that, the present embodiment uses 50 μ L
Concentration is that the Caddy (Cleary) of 100mmol/L replaces 200 μ L concentration in embodiment 1 to be the Caddy (Cleary) of 100mmol/L.
The present invention calculates the fluorescence quantum yield of the cadmium telluride quantum dot that the present embodiment obtains according to technique scheme
(PLQY), result is as in figure 2 it is shown, the fluorescence of Fig. 2 is the embodiment of the present invention 1 and embodiment 9～11 obtains cadmium telluride quantum dot
Quantum yield.In Fig. 2,1 is the fluorescence quantum yield of the cadmium telluride quantum dot that the embodiment of the present invention 9 obtains.As shown in Figure 2, originally
The fluorescence quantum yield of the cadmium telluride quantum dot that embodiment obtains is 11%.
Embodiment 10
Preparing cadmium telluride quantum dot according to the technical scheme in embodiment 1, except for the difference that, the present embodiment uses 400 μ
L concentration is that the Caddy (Cleary) of 100mmol/L replaces 200 μ L concentration in embodiment 1 to be the Caddy (Cleary) of 100mmol/L.
The present invention calculates the fluorescence quantum yield of the cadmium telluride quantum dot that the present embodiment obtains according to technique scheme
(PLQY), result is as in figure 2 it is shown, the fluorescence of Fig. 2 is the embodiment of the present invention 1 and embodiment 9～11 obtains cadmium telluride quantum dot
Quantum yield.In Fig. 2,3 is the fluorescence quantum yield of the cadmium telluride quantum dot that the embodiment of the present invention 10 obtains.As shown in Figure 2, originally
The fluorescence quantum yield of the cadmium telluride quantum dot that embodiment obtains is 20%.
Embodiment 11
Preparing cadmium telluride quantum dot according to the technical scheme in embodiment 1, except for the difference that, the present embodiment uses 600 μ
L concentration is that the Caddy (Cleary) of 100mmol/L replaces 200 μ L concentration in embodiment 1 to be the Caddy (Cleary) of 100mmol/L.
The present invention calculates the fluorescence quantum yield of the cadmium telluride quantum dot that the present embodiment obtains according to technique scheme
(PLQY), result is as in figure 2 it is shown, the fluorescence of Fig. 2 is the embodiment of the present invention 1 and embodiment 9～11 obtains cadmium telluride quantum dot
Quantum yield.In Fig. 2,4 is the fluorescence quantum yield of the cadmium telluride quantum dot that the embodiment of the present invention 9 obtains.As shown in Figure 2, originally
The fluorescence quantum yield of the cadmium telluride quantum dot that embodiment obtains is 12%.
Embodiment 12
Preparing cadmium telluride quantum dot according to the technical scheme in embodiment 1, except for the difference that, the present embodiment is preparing tellurium
During precursor solution, the time of backflow uses 20min to replace the 40min used in embodiment 1.
The present invention calculates the fluorescence quantum yield of the cadmium telluride quantum dot that the present embodiment obtains according to technique scheme
(PLQY), result is as it is shown on figure 3, the fluorescence of Fig. 3 is the embodiment of the present invention 1 and embodiment 12～15 obtains cadmium telluride quantum dot
Quantum yield.In Fig. 3, the value corresponding to abscissa 20 is the fluorescent quantum of the cadmium telluride quantum dot that the embodiment of the present invention 12 obtains
Productivity, from the figure 3, it may be seen that the fluorescence quantum yield of cadmium telluride quantum dot that the present embodiment obtains is 20%.
Embodiment 13
Preparing cadmium telluride quantum dot according to the technical scheme in embodiment 1, except for the difference that, the present embodiment is preparing tellurium
During precursor solution, the time of backflow uses 30min to replace the 40min used in embodiment 1.
The present invention calculates the fluorescence quantum yield of the cadmium telluride quantum dot that the present embodiment obtains according to technique scheme
(PLQY), result is as it is shown on figure 3, the fluorescence of Fig. 3 is the embodiment of the present invention 1 and embodiment 12～15 obtains cadmium telluride quantum dot
Quantum yield.In Fig. 3, the value corresponding to abscissa 30 is the fluorescent quantum of the cadmium telluride quantum dot that the embodiment of the present invention 13 obtains
Productivity, the value corresponding to abscissa 40 is the fluorescence quantum yield of the cadmium telluride quantum dot that the embodiment of the present invention 1 obtains, by Fig. 3
Understanding, the fluorescence quantum yield of the cadmium telluride quantum dot that the present embodiment obtains is 46%.
Embodiment 14
Preparing cadmium telluride quantum dot according to the technical scheme in embodiment 1, except for the difference that, the present embodiment is preparing tellurium
During precursor solution, the time of backflow uses 50min to replace the 40min used in embodiment 1.
The present invention calculates the fluorescence quantum yield of the cadmium telluride quantum dot that the present embodiment obtains according to technique scheme
(PLQY), result is as it is shown on figure 3, the fluorescence of Fig. 3 is the embodiment of the present invention 1 and embodiment 12～15 obtains cadmium telluride quantum dot
Quantum yield.In Fig. 3, the value corresponding to abscissa 50 is the fluorescent quantum of the cadmium telluride quantum dot that the embodiment of the present invention 14 obtains
Productivity, from the figure 3, it may be seen that the fluorescence quantum yield of cadmium telluride quantum dot that the present embodiment obtains is 28%.
Embodiment 15
Preparing cadmium telluride quantum dot according to the technical scheme in embodiment 1, except for the difference that, the present embodiment is preparing tellurium
During precursor solution, the time of backflow uses 60min to replace the 40min used in embodiment 1.
The present invention calculates the fluorescence quantum yield of the cadmium telluride quantum dot that the present embodiment obtains according to technique scheme
(PLQY), result is as it is shown on figure 3, the fluorescence of Fig. 3 is the embodiment of the present invention 1 and embodiment 12～15 obtains cadmium telluride quantum dot
Quantum yield.In Fig. 3, the value corresponding to abscissa 60 is the fluorescent quantum of the cadmium telluride quantum dot that the embodiment of the present invention 15 obtains
Productivity, from the figure 3, it may be seen that the fluorescence quantum yield of cadmium telluride quantum dot that the present embodiment obtains is 26%.
Embodiment 16
Preparing cadmium telluride quantum dot according to the technical scheme in embodiment 1, except for the difference that, the present embodiment is preparing tellurium
During cadmium quantum dot, the time of backflow uses 5min to replace the 30min used in embodiment 1.
The cadmium telluride quantum dot that the present embodiment is obtained by the present invention has carried out absorption spectrum detection, and result as shown in Figure 4, is schemed
The abosrption spectrogram of 4 cadmium telluride quantum dots obtained for the embodiment of the present invention 1 and embodiment 16～24.
Embodiment 17
Preparing cadmium telluride quantum dot according to the technical scheme in embodiment 1, except for the difference that, the present embodiment is preparing tellurium
During cadmium quantum dot, the time of backflow uses 15min to replace the 30min used in embodiment 1.
The cadmium telluride quantum dot that the present embodiment is obtained by the present invention has carried out absorption spectrum detection, and result as shown in Figure 4, is schemed
The abosrption spectrogram of 4 cadmium telluride quantum dots obtained for the embodiment of the present invention 1 and embodiment 16～24.
The cadmium telluride quantum dot that the present embodiment is obtained by the present invention has carried out fluorescence spectrum detection, and result is as it is shown in figure 5, scheme
The fluorescence spectrum figure of 5 cadmium telluride quantum dots obtained for the embodiment of the present invention 17,22 and 24.In Fig. 5, curve 1 is that the present invention is real
Execute the fluorescent spectrum curve of the cadmium telluride quantum dot that example 17 obtains.As shown in Figure 5, the cadmium telluride quantum dot that the present embodiment obtains
Fluorescence emission wavelengths is 532nm.
Embodiment 18
Preparing cadmium telluride quantum dot according to the technical scheme in embodiment 1, except for the difference that, the present embodiment is preparing tellurium
During cadmium quantum dot, the time of backflow uses 40min to replace the 30min used in embodiment 1.
The cadmium telluride quantum dot that the present embodiment is obtained by the present invention has carried out absorption spectrum detection, and result as shown in Figure 4, is schemed
The abosrption spectrogram of 4 cadmium telluride quantum dots obtained for the embodiment of the present invention 1 and embodiment 16～24.
Embodiment 19
Preparing cadmium telluride quantum dot according to the technical scheme in embodiment 1, except for the difference that, the present embodiment is preparing tellurium
During cadmium quantum dot, the time of backflow uses 50min to replace the 30min used in embodiment 1.
The cadmium telluride quantum dot that the present embodiment is obtained by the present invention has carried out absorption spectrum detection, and result as shown in Figure 4, is schemed
The abosrption spectrogram of 4 cadmium telluride quantum dots obtained for the embodiment of the present invention 1 and embodiment 16～24.
Embodiment 20
Preparing cadmium telluride quantum dot according to the technical scheme in embodiment 1, except for the difference that, the present embodiment is preparing tellurium
During cadmium quantum dot, the time of backflow uses 60min to replace the 30min used in embodiment 1.
The cadmium telluride quantum dot that the present embodiment is obtained by the present invention has carried out absorption spectrum detection, and result as shown in Figure 4, is schemed
The abosrption spectrogram of 4 cadmium telluride quantum dots obtained for the embodiment of the present invention 1 and embodiment 16～24.
Embodiment 21
Preparing cadmium telluride quantum dot according to the technical scheme in embodiment 1, except for the difference that, the present embodiment is preparing tellurium
During cadmium quantum dot, the time of backflow uses 80min to replace the 30min used in embodiment 1.
The cadmium telluride quantum dot that the present embodiment is obtained by the present invention has carried out absorption spectrum detection, and result as shown in Figure 4, is schemed
The abosrption spectrogram of 4 cadmium telluride quantum dots obtained for the embodiment of the present invention 1 and embodiment 16～24.
Embodiment 22
Preparing cadmium telluride quantum dot according to the technical scheme in embodiment 1, except for the difference that, the present embodiment is preparing tellurium
During cadmium quantum dot, the time of backflow uses 120min to replace the 30min used in embodiment 1.
The cadmium telluride quantum dot that the present embodiment is obtained by the present invention has carried out absorption spectrum detection, and result as shown in Figure 4, is schemed
The abosrption spectrogram of 4 cadmium telluride quantum dots obtained for the embodiment of the present invention 1 and embodiment 16～24.
The cadmium telluride quantum dot that the present embodiment is obtained by the present invention has carried out fluorescence spectrum detection, and result is as it is shown in figure 5, scheme
The fluorescence spectrum figure of 5 cadmium telluride quantum dots obtained for the embodiment of the present invention 17,22 and 24.In Fig. 5, curve 2 is that the present invention is real
Execute the fluorescent spectrum curve of the cadmium telluride quantum dot that example 22 obtains.As shown in Figure 5, the cadmium telluride quantum dot that the present embodiment obtains
Fluorescence emission wavelengths is 610nm.
Embodiment 23
Preparing cadmium telluride quantum dot according to the technical scheme in embodiment 1, except for the difference that, the present embodiment is preparing tellurium
During cadmium quantum dot, the time of backflow uses 350min to replace the 30min used in embodiment 1.
The cadmium telluride quantum dot that the present embodiment is obtained by the present invention has carried out absorption spectrum detection, and result as shown in Figure 4, is schemed
The abosrption spectrogram of 4 cadmium telluride quantum dots obtained for the embodiment of the present invention 1 and embodiment 16～24.
Embodiment 24
Preparing cadmium telluride quantum dot according to the technical scheme in embodiment 1, except for the difference that, the present embodiment is preparing tellurium
During cadmium quantum dot, the time of backflow uses 750min to replace the 30min used in embodiment 1.
The cadmium telluride quantum dot that the present embodiment is obtained by the present invention has carried out absorption spectrum detection, and result as shown in Figure 4, is schemed
The abosrption spectrogram of 4 cadmium telluride quantum dots obtained for the embodiment of the present invention 1 and embodiment 16～24.In Fig. 4, have 10 songs
Line, is followed successively by the cadmium telluride quantum dot that the embodiment of the present invention 16,17,1,18,19,20,21,22,23 and 24 obtains from left to right
Absorption spectrum curve.
The cadmium telluride quantum dot that the present embodiment is obtained by the present invention has carried out fluorescence spectrum detection, and result is as it is shown in figure 5, scheme
The fluorescence spectrum figure of 5 cadmium telluride quantum dots obtained for the embodiment of the present invention 17,22 and 24.In Fig. 5, curve 3 is that the present invention is real
Execute the fluorescent spectrum curve of the cadmium telluride quantum dot that example 24 obtains.As shown in Figure 5, the cadmium telluride quantum dot that the present embodiment obtains
Fluorescence emission wavelengths is 670nm.
As can be seen from the above embodiments, the preparation method of the cadmium telluride quantum dot that the present invention provides not only reacts gentle,
And cost is relatively low, and the cadmium telluride quantum dot fluorescence quantum yield obtained is the highest.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For Yuan, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (5)
1. a preparation method for cadmium telluride quantum dot, comprises the following steps:
A) sodium bisulphite formaldehyde, tellurium simple substance and water are mixed in the basic conditions, react, obtain tellurium precursor；
B) in oxygen-free environment, by cadmium source, TGA and described step A) the tellurium precursor that obtains mixes, reacts, obtain
Cadmium telluride quantum dot；
The mol ratio of described sodium bisulphite formaldehyde and tellurium simple substance is (10～20): 1, rubbing of described cadmium source and described TGA
That ratio is 1:(0.5～5), the mol ratio in described tellurium simple substance and cadmium source is 0.5:(0.25～3)；
Described step B) in reaction under reflux conditions carry out, the temperature of described reaction is 90～110 DEG C, the time of described reaction
It is 5～750min.
Preparation method the most according to claim 1, it is characterised in that described step A) in reaction under reflux conditions enter
OK；
Described step A) in reaction temperature be 90～110 DEG C；
Described step A) in reaction time be 20～60min.
Preparation method the most according to claim 1, it is characterised in that described step B) specifically include following steps:
Cadmium source, TGA and alkaline medium are mixed, obtains cadmium precursor；
In oxygen-free environment, described cadmium precursor is mixed with described tellurium precursor, reacts, obtain cadmium telluride quantum dot.
Preparation method the most according to claim 3, it is characterised in that the pH value of described cadmium precursor is 11～12.
Preparation method the most according to claim 3, it is characterised in that described cadmium source includes Caddy (Cleary), cadmium nitrate, cadmium sulfate
With one or more in cadmium perchlorate；
Described alkaline medium includes sodium hydroxide and/or potassium hydroxide.
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