CN103436258A - Method for synthesizing copper-zinc-tin-sulfur quantum dots by utilizing ultrasonic cavitation - Google Patents

Method for synthesizing copper-zinc-tin-sulfur quantum dots by utilizing ultrasonic cavitation Download PDF

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CN103436258A
CN103436258A CN2013103409608A CN201310340960A CN103436258A CN 103436258 A CN103436258 A CN 103436258A CN 2013103409608 A CN2013103409608 A CN 2013103409608A CN 201310340960 A CN201310340960 A CN 201310340960A CN 103436258 A CN103436258 A CN 103436258A
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zinc
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copper
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CN103436258B (en
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常远程
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Shaanxi Coal and Chemical Technology Institute Co Ltd
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Abstract

A method for synthesizing copper-zinc-tin-sulfur quantum dots by utilizing ultrasonic cavitation comprises the following steps: mixing cupric sulfate pentahydrate crystals, zinc sulphate heptahydrate crystals, stannic sulfate dihydrate crystals and thiocarbamide crystals, adding the mixture into ethylene alcohol, and mixing uniformly to obtain a solution A; immersing the probe of an ultrasonic treatment instrument into the solution A, and then separating powder from the solution subjected to treatment by the ultrasonic treatment instrument; finally, washing the powder with n-dodecyl mercaptan so as to remove excessive sulfur ions. With adoption of the method disclosed by the invention, the copper-zinc-tin-sulfur quantum dots are synthesized by utilizing ultrasonic cavitation. The method has the advantages of simple and convenient operation, high repeatability, low cost, controllability of granular size of the copper-zinc-tin-sulfur quantum dots and the like. In addition, no highly toxic chemical substances are used during the whole process, the preparation process is fast, the environmentally friendliness is achieved, and the prepared copper-zinc-tin-sulfur material is pure in phase.

Description

A kind of method of utilizing the synthetic copper-zinc-tin-sulfur nano-quantum point of supersonic gas cavitation
[technical field]
The present invention relates to fluorescent dye biological medical science, novel nano quantum dot solar cell, the fields such as Photoelectrochemistry of semiconductor battery (Photoelectrochemical) solar hydrogen making, particularly a kind ofly utilize the supersonic gas cavitation to synthesize copper-zinc-tin-sulfur (Cu 2znSnS 4) method of nano-quantum point (quantum dot).
[background technology]
The semiconductor material quantum dot is at the nanometer semiconductor structure that conduction band electron, valence band hole and exciton are held onto on three direction in spaces.Electron motion all is restricted at three-dimensional space, therefore sometimes is called as " artificial atom ", " superlattice ", " hyperonic atom " or " quantum dot atom ".This constraint can ascribe to electrostatic potential (by outside electrode, the doping, strain, impurity produces), the interface of two kinds of different semiconductor materials (for example: in certainly organizing quantum dot), semi-conductive surface (for example: semiconductor nanocrystal), or above three's combination.The separative quantized power spectrum of quantum dot tool.Corresponding wave function spatially is arranged in quantum dot, but extends in several lattice period.Quantum dot has electronics, hole or the hole-electron pair of a small amount of (1-100) integer, its with electric weight be the integral multiple of elementary charge.The particle diameter of quantum dot is generally between 1～10nm, and due to electronics and hole, by quantum confinement, continuous energy band structure becomes the discrete energy levels structure with molecular characterization, can emitting fluorescence after being excited.Scientist has invented many diverse ways and has manufactured quantum dot, and expects that this nano material has great application potential on the nanoelectronics of 21st century.
Through more than ten years update, set up so far the preparation method of multiple quantum dot, mainly contain physical method and chemical process, be chemically main.At present, the metal organic synthesis method of quantum dot is to use the earliest, the most a kind of method.The research of quantum dot be the nineties in 20th century the earliest the cadmium selenide from be embedded in glass (CdSe) quantum dot start.Report dimethyl cadmium (Cd (CH is arranged in 1993 3) 2), trioctylphosphine selenizing phosphine (SeTOP) is as precursor, trioctyl phosphine oxide (TOPO), as ligand solvent, has synthesized the CdSe quantum dots of High Efficiency Luminescence, because the CdSe nano particle is insoluble to methyl alcohol, can add excessive methanol, by centrifugation, obtain the CdSe nano particle.But whole complex technical process, used the highly toxic material heavy metal cadmium, thereby its extensive use is restricted.
The quaternary compound that copper-zinc-tin-sulfur is the stannite structure, its energy gap (Eg) is 1.51 electron-volts.It is direct band-gap semicondictor and has higher uptake factor and (be greater than 10 4cm -1).The copper-zinc-tin-sulfur material cost is very low, and all elements in the earth's crust, all reserves are huge, and the nontoxic pollution-free of material own, be a kind of photovoltaic material that has development prospect.Have not yet to see the report of synthetic this kind of material nano quantum dot.Therefore, the synthesis technique of researching and developing new nontoxic low-cost copper-zinc-tin-sulfur nano-quantum point has very important using value.
[summary of the invention]
The technical problem to be solved in the present invention is to provide a kind of method of utilizing the synthetic copper-zinc-tin-sulfur nano-quantum point of supersonic gas cavitation, with low cost, easy and simple to handle, high, the surface charge of repeatability and surface properties are controlled, whole technological process is not used hypertoxic chemical substance, preparation process speed is fast, environmentally friendly.
The technical solution adopted in the present invention is as follows:
A kind of method of utilizing the synthetic copper-zinc-tin-sulfur nano-quantum point of supersonic gas cavitation, by the cupric sulfate pentahydrate crystal, the Zinc Sulphate Heptahydrate crystal, sulfate dihydrate tin crystal and thiocarbamide crystal join in ethylene glycol after mixing, obtain solution A after mixing, the probe of ultrasonication instrument is immersed in solution A, then, solution separating after the ultrasonication instrument is processed goes out powder, finally powder is got final product after n-dodecyl mercaptan washs to remove unnecessary sulfonium ion.
As the preferred embodiments of the present invention, described cupric sulfate pentahydrate crystal, the Zinc Sulphate Heptahydrate crystal, sulfate dihydrate tin crystal and thiocarbamide crystal be take mol ratio and are taken as 2:1:1:4.
Described cupric sulfate pentahydrate crystal, Zinc Sulphate Heptahydrate crystal, sulfate dihydrate tin crystal, thiocarbamide crystal, and ethylene glycol is analytical pure purity.
Described solution A is for take the solution that volumetric molar concentration that zinc sulfate is standard is 5-15 mM/l.
The probe of described ultrasonication instrument is immersed in 2-6 centimetre under the solution A liquid level.
The power of described ultrasonication instrument is 100-300 watt, and frequency is the 10-30 kilohertz, and the opening time of ultrasonication instrument is 2-10 minute.
The opening time of described ultrasonication instrument is 6-10 minute.
The opening time of described ultrasonication instrument is 6 minutes.
Compared with prior art, the present invention at least has following beneficial effect: in the methods of the invention, cupric sulfate pentahydrate crystal, Zinc Sulphate Heptahydrate crystal and sulfate dihydrate tin crystal dissolve readily in ethylene glycol, produce a large amount of Cu 2+, Zn 2+and Sn 2+, thiocarbamide (CH 4n 2s) crystal slowly is decomposed into S under hyperacoustic effect 2-, along with the unlatching of ultrasonication instrument, increasing S is arranged 2-produce.Cu 2+, Zn 2+, Sn 2+and S 2-synthetic copper-zinc-tin-sulfur nano-quantum point under the strong effect of ultrasonic excitation air pocket.The inventive method utilizes the supersonic gas cavitation to synthesize the copper-zinc-tin-sulfur nano-quantum point.The advantage such as that the method has is easy and simple to handle, repeatability is high, cost is low, the nano-quantum point granular size is controlled.Because the nano-quantum point granular size is controlled, thereby can comparatively be easy to regulate the band gap width of quanta point material, synthesize the copper-zinc-tin-sulfur nano-quantum point material that there is the huge applications prospect in solar hydrogen making and quantum dot solar cell field.Whole technological process is not used hypertoxic chemical substance in addition, and preparation process speed is fast, environmentally friendly, and the phase of the copper-zinc-tin-sulfur material made is pure.
[accompanying drawing explanation]
Fig. 1 is the inventive method composition principle figure.
Fig. 2 (a) and figure (b) are respectively the transmission electron microscope schematic diagram according to embodiment 1 and embodiment 2 products obtained therefroms, and Fig. 2 (c) and Fig. 2 (d) are respectively the nano particle diameter Distribution figure according to embodiment 1 and embodiment 2 products obtained therefroms.
Fig. 3 (a) and figure (b) are respectively the transmission electron microscope schematic diagram according to embodiment 3 and embodiment 4 products obtained therefroms, and Fig. 3 (c) and Fig. 3 (d) are respectively the nano particle diameter Distribution figure according to embodiment 3 and embodiment 4 products obtained therefroms.
Fig. 4 is according to the absorption curve of embodiment 2,3,4 products obtained therefroms (Tauc figure) comparison diagram.
Fig. 5 is after dropping in ITO and do on the surface-treated conductive glass according to embodiment 3 products obtained therefroms, the structural representation of copper-zinc-tin-sulfur nano-quantum point and ITO nano particle.
Fig. 6 is the Raman Measurement collection of illustrative plates of the inventive method products obtained therefrom.
[embodiment]
During in liquid, can excite air pocket (Cavitation) phenomenon when the frequency ul-trasonic irradiation that is 20～50 kilo hertzs, comprise the growing up and explosion three steps of microvesicle of appearance, microvesicle of gas core.Under ultrasonication, fluid produces motion sharply, due to the variation of acoustic pressure, solvent is compressed and rarefaction, and at the sparse phase region of sound wave, air pocket expands and grows up, and liquid vapors or gas around being are full of.At the compression phase region, air pocket subsides very soon, breaks, and produces a large amount of microvesicles, and they can be used as again new gas core.The ultrasonic impact on chemical reaction, its major cause is exactly that these microvesicles can produce very strong shockwave when growing up so that break suddenly.When the microvesicle explosion, can in local space, produce high temperature and 2000 atmospheric high pressure up to 5000 ℃.This extreme environment can induce series of chemical, comprises metallographic phase shift reaction, the reaction of solid-liquid two-phase interface, polymerization and degradation of polymer reaction etc., also can greatly promote generation and the growth of semiconductor microcrystalline simultaneously.
The present invention utilizes the method for the synthetic copper-zinc-tin-sulfur nano-quantum point of supersonic gas cavitation to comprise the following steps:
Step 1, by the cupric sulfate pentahydrate crystal of analytical pure purity, Zinc Sulphate Heptahydrate crystal, sulfate dihydrate tin crystal, thiocarbamide (CH 4n 2s) crystal be take the ratio that mol ratio is 2:1:1:4 and is weighed.
Step 2, the crystal that will be weighed by step 1 mix, and join in the ethylene glycol of 15-30 milliliter analytical pure purity, make to take the solution that volumetric molar concentration that zinc sulfate is standard is 5-15 mM/l, and solution is oyster white, the called after solution A.
Step 3, the solution that step 2 is made are contained in flask, flask are placed on the table top of laboratory ultrasonication instrument.Adjust the height of ultrasonication instrument probe, make probe be immersed in 2-6 centimetre under liquid level.
Step 4, the power that the ultrasonication instrument is set are 100-300 watt, and frequency is the 10-30 kilohertz, open the ultrasonication instrument 2 minutes, obtain solution B.
Step 5, the solution B that step 4 is obtained are separated (centrifuge speed 2000-6000 rev/min opens 3-8 minute) with whizzer, obtain powder.N-dodecyl mercaptan (CH by analytical pure purity 3(CH 2) 10CH 2sH) the repetitive scrubbing powder is 3-6 time.N-dodecyl mercaptan can be removed unnecessary sulfonium ion, and effectively disperses the copper-zinc-tin-sulfur nano-quantum point.
Can obtain copper-zinc-tin-sulfur nano-quantum point solution (n-dodecyl mercaptan is solvent) after step 6, washing.
Embodiment 1:
Step 1, by 0.4 mmole cupric sulfate pentahydrate crystal of analytical pure purity, the 0.2 milli Zinc Sulphate Heptahydrate crystal that rubs, 0.2 milli sulfate dihydrate tin crystal and the 0.8 milli thiocarbamide (CH that rubs that rubs 4n 2s) crystal joins in the ethylene glycol of 20 milliliters of analytical pure purity, makes to take the solution that volumetric molar concentration that zinc sulfate is standard is 10 mM/ls, and solution is oyster white, the called after solution A.
Step 2, whizzer for solution A is separated to (4000 rev/mins of centrifuge speeds are opened 3 minutes), obtain white powder.N-dodecyl mercaptan (CH by analytical pure purity 3(CH 2) 10CH 2sH) the repetitive scrubbing powder is 6 times.
Can obtain copper-zinc-tin-sulfur nano-quantum point solution (n-dodecyl mercaptan is solvent) after step 6, washing.
Embodiment 2
Step 1, by 0.2 mmole cupric sulfate pentahydrate crystal of analytical pure purity, the 0.1 milli Zinc Sulphate Heptahydrate crystal that rubs, 0.1 milli sulfate dihydrate tin crystal and the 0.4 milli thiocarbamide (CH that rubs that rubs 4n 2s) crystal joins in the ethylene glycol of 30 milliliters of analytical pure purity, makes to take the solution that volumetric molar concentration that zinc sulfate is standard is 5 mM/ls, and solution is oyster white, the called after solution A.
Step 2, the solution A that step 1 is made are contained in 50 ml flasks, flask are placed on the table top of laboratory ultrasonication instrument.Adjust the height of ultrasonication instrument probe, make probe be immersed under liquid level 2 centimetres.
Step 3, the power that the ultrasonication instrument is set are 300 watts, and frequency is 10 kilohertzs, open the ultrasonication instrument 2 minutes, obtain solution B.
Step 4, whizzer for solution B is separated to (2000 rev/mins of centrifuge speeds are opened 3-8 minute), obtain orange powder.N-dodecyl mercaptan (CH by analytical pure purity 3(CH 2) 10CH 2sH) repetitive scrubbing powder.
Can obtain copper-zinc-tin-sulfur nano-quantum point solution (n-dodecyl mercaptan is solvent) after step 5, washing.
Embodiment 3
Step 1, by 0.4 mmole cupric sulfate pentahydrate crystal of analytical pure purity, the 0.2 milli Zinc Sulphate Heptahydrate crystal that rubs, 0.2 milli sulfate dihydrate tin crystal and the 0.8 milli thiocarbamide (CH that rubs that rubs 4n 2s) crystal joins in the ethylene glycol of 15 milliliters of analytical pure purity, makes to take the solution that volumetric molar concentration that zinc sulfate is standard is 10 mM/ls, and solution is oyster white, the called after solution A.
Step 2,, the solution A that step 1 is made is contained in 50 ml flasks, flask is placed on the table top of laboratory ultrasonication instrument.Adjust the height of ultrasonication instrument probe, make probe be immersed under liquid level 4 centimetres.
Step 3, the power that the ultrasonication instrument is set are 100 watts, and frequency is 30 kilohertzs, open the ultrasonication instrument 6 minutes, obtain solution C.
Step 4, whizzer for solution C is separated to (4500 rev/mins of centrifuge speeds are opened 6 minutes), obtain red powder.N-dodecyl mercaptan (CH by analytical pure purity 3(CH 2) 10CH 2sH) the repetitive scrubbing powder is 6 times.
Can obtain copper-zinc-tin-sulfur nano-quantum point solution (n-dodecyl mercaptan is solvent) after step 5, washing.
Embodiment 4
Step 1, by 0.4 mmole cupric sulfate pentahydrate crystal of analytical pure purity, the 0.2 milli Zinc Sulphate Heptahydrate crystal that rubs, 0.2 milli sulfate dihydrate tin crystal and the 0.8 milli thiocarbamide (CH that rubs that rubs 4n 2s) crystal joins in the ethylene glycol of 25 milliliters of analytical pure purity, makes to take the solution that volumetric molar concentration that zinc sulfate is standard is 15 mM/ls, and solution is oyster white, the called after solution A.
Step 2,, the solution A that step 1 is made is contained in 50 ml flasks, flask is placed on the table top of laboratory ultrasonication instrument.Adjust the height of ultrasonication instrument probe, make probe be immersed under liquid level 6 centimetres.
Step 3, the power that the ultrasonication instrument is set are 200 watts, and frequency is 15 kilohertzs, open the ultrasonication instrument 10 minutes, obtain solution D.
Step 4, whizzer for solution D is separated to (6000 rev/mins of centrifuge speeds are opened 3-8 minute), obtain brown ceramic powder.N-dodecyl mercaptan (CH by analytical pure purity 3(CH 2) 10CH 2sH) the repetitive scrubbing powder is 6 times.
Can obtain copper-zinc-tin-sulfur nano-quantum point solution (n-dodecyl mercaptan is solvent) after step 5, washing.
Cupric sulfate pentahydrate crystal, Zinc Sulphate Heptahydrate crystal and sulfate dihydrate tin crystal dissolve readily in ethylene glycol, produce a large amount of Cu 2+, Zn 2+and Sn 2+, thiocarbamide (CH 4n 2s) crystal slowly is decomposed into S under hyperacoustic effect 2-, the time of opening along with the ultrasonication instrument was increased to 10 minutes by 2 minutes, and increasing S is arranged 2-produce.Cu 2+, Zn 2+, Sn 2+and S 2-synthetic copper-zinc-tin-sulfur nano-quantum point under the strong effect of ultrasonic excitation air pocket.The cavitation time is longer, and it is more that the thiocarbamide crystal decomposes, S in solution 2-more, the time that the copper-zinc-tin-sulfur nano-quantum point is grown up is just longer, and the mean sizes of quantum dot is just larger.Therefore the opening time of adjusting the ultrasonication instrument just can be controlled the particle size of copper-zinc-tin-sulfur nano-quantum point, be reflected in solution A, B, C, the D of each embodiment, the color relation of solution becomes orange by white (particle diameter minimum), red and brown (particle diameter maximum), as shown in Figure 1.The mean diameter that transmission electron microscope (TEM) is measured the copper-zinc-tin-sulfur nano-quantum point that shows solution A, B, C, D is respectively 2,4,8 and 10 nanometers, as shown in Figure 2,3.
Due to the quantum confinement effect of nano-quantum point, the quantum dot that particle is little shows more shallow color and larger band gap width, and the quantum dot that particle is large shows darker color and less band gap width.Transmittance/reflectance is measured the band gap width that shows solution B, C, D copper-zinc-tin-sulfur nano-quantum point and is respectively 2.4,2.0 and 1.6 electron-volts (as Fig. 4).Wherein the band gap width of solution C and solution D is (2.0 electron-volts, 1.6 electron-volt) meet fully with the photoelectrochemical cell material required in theory and the optimum energy gap of solar cell material, so this class nano-quantum point has extremely bright application prospect at solar hydrogen making and quantum dot solar cell field.
As everyone knows, in the research field of photoelectrochemical cell solar hydrogen making, choosing of optoelectronic pole material is an insoluble problem always.The band gap width of desired light electrode materials must be 2.0 electron-volts.Copper-zinc-tin-sulfur nano-quantum point material in solution C meets this requirement, solution C can be dropped in by nano indium tin metal oxide (ITO) and do on the surface-treated conductive glass.The copper-zinc-tin-sulfur nano-quantum point can be attached to the ITO nano particle like this, the optoelectronic pole with such structure as photoelectrochemical cell, thus can realize that effective contact area is far longer than real area (Fig. 5).
Fine (as Fig. 6) that the Raman Measurement collection of illustrative plates (Raman) of crystal grain and the data (Femandes 2011) of having reported meet, and the phase of copper-zinc-tin-sulfur material is pure, not containing being easy to the impurity such as zinc sulphide that occur in common plasma sputtering technique.
Beneficial effect:
Through more than ten years update, set up so far the preparation method of multiple quantum dot, mainly contain physical method and chemical process, be chemically main.Using dimethyl cadmium and trioctylphosphine selenizing phosphine as precursor, and trioctyl phosphine oxide, as ligand solvent, adopts metal organic synthesis method to successfully synthesize the CdSe quantum dots of High Efficiency Luminescence.
As a kind of overcast, high-level efficiency photochromics that has application prospect, copper-zinc-tin-sulfur has higher uptake factor, and the nontoxic pollution-free of material own, is the study hotspot of area of solar cell already.
Beneficial effect of the present invention is: explored first a Technology Ways that utilizes the synthetic copper-zinc-tin-sulfur nano-quantum point of supersonic gas cavitation.The advantage such as that the method has is easy and simple to handle, repeatability is high, cost is low, the nano-quantum point granular size is controlled.Special needs to be pointed out is, because the nano-quantum point granular size is controlled, thereby can comparatively be easy to regulate the band gap width of quanta point material, synthesize the copper-zinc-tin-sulfur nano-quantum point material that there is the huge applications prospect in solar hydrogen making and quantum dot solar cell field.Whole technological process is not used hypertoxic chemical substance in addition, and preparation process speed is fast, environmentally friendly, and the phase of the copper-zinc-tin-sulfur material made is pure.
Adopt the synthetic copper-zinc-tin-sulfur nano-quantum point of the inventive method, can be used as the fluorescence dye luminous marker, in research fields such as biological chemistry, molecular biology, cytobiology, genomics, proteomics, drug screenings, there is great application prospect.The copper-zinc-tin-sulfur nano-quantum point can be by controlling shape, structure and the size of quantum dot, regulate easily its energy gap width, thereby can also be widely used in the fields such as novel nano quantum dot solar cell (theoretical electricity conversion is up to 70%) and Photoelectrochemistry of semiconductor battery solar hydrogen making.

Claims (8)

1. a method of utilizing the synthetic copper-zinc-tin-sulfur nano-quantum point of supersonic gas cavitation, it is characterized in that: by the cupric sulfate pentahydrate crystal, the Zinc Sulphate Heptahydrate crystal, sulfate dihydrate tin crystal and thiocarbamide crystal join in ethylene glycol after mixing, obtain solution A after mixing, the probe of ultrasonication instrument is immersed in solution A, then, solution separating after the ultrasonication instrument is processed goes out powder, finally powder is got final product after n-dodecyl mercaptan washs to remove unnecessary sulfonium ion.
2. a kind of method of utilizing the synthetic copper-zinc-tin-sulfur nano-quantum point of supersonic gas cavitation as claimed in claim 1, it is characterized in that: described cupric sulfate pentahydrate crystal, the Zinc Sulphate Heptahydrate crystal, sulfate dihydrate tin crystal and thiocarbamide crystal be take mol ratio and are taken as 2:1:1:4.
3. a kind of method of utilizing the synthetic copper-zinc-tin-sulfur nano-quantum point of supersonic gas cavitation as claimed in claim 1, it is characterized in that: described cupric sulfate pentahydrate crystal, Zinc Sulphate Heptahydrate crystal, sulfate dihydrate tin crystal, thiocarbamide crystal, and ethylene glycol is analytical pure purity.
4. a kind of method of utilizing the synthetic copper-zinc-tin-sulfur nano-quantum point of supersonic gas cavitation as claimed in claim 1 is characterized in that: described solution A is for take the solution that volumetric molar concentration that zinc sulfate is standard is 5-15 mM/l.
5. a kind of method of utilizing the synthetic copper-zinc-tin-sulfur nano-quantum point of supersonic gas cavitation as claimed in claim 1, it is characterized in that: the probe of described ultrasonication instrument is immersed in 2-6 centimetre under the solution A liquid level.
6. a kind of method of utilizing the synthetic copper-zinc-tin-sulfur nano-quantum point of supersonic gas cavitation as described as any one in claim 1 to 5, it is characterized in that: the power of described ultrasonication instrument is 100-300 watt, frequency is the 10-30 kilohertz, and the opening time of ultrasonication instrument is 2-10 minute.
7. a kind of method of utilizing the synthetic copper-zinc-tin-sulfur nano-quantum point of supersonic gas cavitation as described as any one in claim 6, it is characterized in that: the opening time of described ultrasonication instrument is 6-10 minute.
8. a kind of method of utilizing the synthetic copper-zinc-tin-sulfur nano-quantum point of supersonic gas cavitation as described as any one in claim 6, it is characterized in that: the opening time of described ultrasonication instrument is 6 minutes.
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