CN103214029A - Preparation method of wurtzite CuInS2 nanodisk - Google Patents

Preparation method of wurtzite CuInS2 nanodisk Download PDF

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CN103214029A
CN103214029A CN2013101461975A CN201310146197A CN103214029A CN 103214029 A CN103214029 A CN 103214029A CN 2013101461975 A CN2013101461975 A CN 2013101461975A CN 201310146197 A CN201310146197 A CN 201310146197A CN 103214029 A CN103214029 A CN 103214029A
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wurtzite
solution
cuins
preparation
nanometer plate
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陈勤妙
周芳芳
窦晓鸣
李振庆
倪一
陈进
王婷婷
庄松林
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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Abstract

The invention provides a preparation method of a wurtzite CuInS2 nanodisk. The preparation method is characterized by comprising the following steps of: sufficiently dissolving CuCl2*2H2O and InCl3*4H2O in diethylene glycol to obtain first solution, and sufficiently dissolving SC(NH2)2 in diethylene glycol to obtain solution 2; heating the first solution to 180 DEG C in an anhydrous and oxygen-free environment, adding (HOCH2CH2)3N liquid at first, and mixing the first solution with the second solution to obtain third solution; reacting the third solution under the protection of nitrogen at 180 DEG C for 30-240min, and after reacting, naturally cooling to room temperature to obtain mixed solution; and separating and drying the obtained mixed solution to obtain the wurtzite CuInS2 nanodisk. According to the invention, by adding proper complexing agent, the wurtzite CuInS2 nanodisk, namely TEA (Tri Ethyl Amine), is obtained; and the wurtzite CuInS2 nanodisk is high in stability and has wide-band tunable nanometer level.

Description

Wurtzite CuInS 2The preparation method of nanometer plate
Technical field
The present invention relates to a kind of compound film solar battery obsorbing layer wurtzite CuInS 2The preparation method of nanometer plate.
Background technology
Thin-film solar cells has the transformation efficiency height, energy consumption is hanged down characteristics such as reaching stable height, meets solar battery thin filmization, big areaization, high efficiency development trend, is considered to be the low-cost substitute technology of conventional solar cell.The key of thin-film solar cells transformation efficiency height is the technology of preparing of absorption layer, and the current major technique that is used for synthetic CIGS absorbing layer of thin film solar cell: the chemical vapor transportation of vacuum-evaporation, magnetron sputtering, galvanic deposit, electron beam evaporation, plating, enclosed space, chemical vapour deposition, molecular beam epitaxy, Metalorganic chemical vapor deposition method etc. all belong to the vacuum preparation method.Though vacuum production method can obtain efficiency of conversion higher solar energy battery, however also exist many defectives as: vacuum apparatus costs an arm and a leg, and the low and settling rate of material rate of utilization is low etc.In recent years, antivacuum preparation technology because of have low cost, easy to operate, potential advantages have obtained a large amount of research and developments easily to realize that big area is commercially produced etc.Wherein, silk screen print method is a kind of extremely important and efficient is high and technology that cost is low: with CuInS 2Preparation of nanoparticles becomes the printing slurry, and printing forms the absorption layer film on substrate of glass then, at last it is annealed in nitrogen environment to improve the absorption layer quality of forming film.In silk screen printing, synthetic high-quality CuInS 2Nano particle is very crucial, therefore emerges many synthetic CuInS 2The technology of nano particle is as hydrothermal method, thermal decomposition method and hot injection method.Hot injection method is simple and efficient, has been subjected to people's favor in nanometer is synthetic gradually.CuInS 2Compound is a kind of important CIGS compound, and it mainly contains three kinds and has form: yellow copper structure, zink sulphide and wurtzite.Wurzite structure is metastable at normal temperatures, is easy to just become yellow copper structure; In addition, wurtzite shows good handiness aspect stoichiometric ratio, and this excellent characteristic can ascribe different copper atoms to and phosphide atom is shared a lattice site.This special structural characteristics of wurtzite makes CuInS 2Can in the scope of a broad, carry out the adjusting of fermi level, significant to high performance solar batteries.Therefore, the Wurzite structure CuInS of synthesizing stable at normal temperatures 2It is extremely important just to seem.And synthon zinc ore structure C uInS commonly used at present 2Method adopt material such as oleyl amines as the method for treat different things alike (one-pot) etc., and the common synthesis temperature of these methods all can be higher than 220 oC, this material has certain corrodibility to skin simultaneously, can cause serious skin burn and ocular injury, and very big to hydrobiont toxicity, so this waste liquid cannot directly discharge, must process handle.
In sum, but how by a kind of simple and low temperature is realized, hot injection method prepares the CuInS of stable Wurzite structure safely and efficiently 2Significant to the photovoltaic field.
Summary of the invention
The object of the present invention is to provide a kind of wurtzite CuInS 2The preparation method of nanometer plate is to overcome the above-mentioned shortcoming and defect of existing in prior technology.
The invention provides a kind of wurtzite CuInS 2The preparation method of nanometer plate is characterized in that, may further comprise the steps:
Steps A. with CuCl 22H 2O and InCl 34H 2O fully is dissolved in glycol ether and obtains solution one, with SC (NH 2) 2Fully be dissolved in glycol ether and obtain solution two;
Step B. is heated to 180 ℃ with solution one in the anhydrous and oxygen-free environment, add (HOCH earlier 2CH 2) 3N liquid mixes obtaining solution three again with solution two;
Step C. solution three reacts under 180 ℃ of temperature and protection of nitrogen gas, and the reaction times is 30～240 minutes, naturally cools to room temperature after reaction finishes and obtains mixing solutions;
Step D. separates drying with the gained mixing solutions, obtains Wurzite structure CuInS 2Nanometer plate;
Wherein, described CuCl 2.2H 2O amount of substance: InCl 3.4H 2O amount of substance: SC (NH 2) 2Amount of substance: (HOCH 2CH 2) 3The ratio of N volume is 1mol:1 mol:4 mol:3L.
In addition, the invention provides a kind of wurtzite CuInS 2The preparation method of nanometer plate can also have such feature: fully carry out magnetic agitation in the dissolved process in the steps A.
In addition, the invention provides a kind of wurtzite CuInS 2The preparation method of nanometer plate can also have such feature: the anhydrous and oxygen-free environment is to realize by alternately vacuumizing and feed nitrogen among the step B.
In addition, the invention provides a kind of wurtzite CuInS 2The preparation method of nanometer plate can also have such feature: the reaction times is 150 min among the step C.
Further, the invention provides a kind of wurtzite CuInS 2The preparation method of nanometer plate can also have the described separation drying of such feature: step D and may further comprise the steps:
D1. after in mixing solutions, adding alcohol, separate acquisition initial precipitation thing with whizzer;
D2. after in the initial precipitation thing, adding alcohol, separate the acquisition throw out with whizzer;
D3. repeating step D2 is three to five times, obtains final throw out;
D4. after in final throw out, adding an amount of alcohol, in loft drier, carry out drying, obtain Wurzite structure CuInS 2Nanometer plate.
The effect and the effect of invention
According to wurtzite CuInS provided by the invention 2The preparation method of nanometer plate is a kind of gentleness relatively and the solvent of environmental protection because solvent uses glycol ether, and it has colourless, odorless, transparent, hygroscopic thick liquid, pungent sweet taste is arranged, non-corrosiveness, low toxicity.245 ℃ of boiling points, fusing point-6.5 ℃, zero pour-10.45 ℃, flash-point 123.9, specific refractory power 1.4472, relative density 1.1184, viscosity 0.30 pool, so other polar solvents such as soluble in water, pure, acetone, ether, ethylene glycol are its excellent property; And glycol ether is compared with oleyl amine, and its price is also relatively cheap.So, can realize preparation wurtzite CuInS under 180 ℃ of conditions of lower temperature 2Nanometer plate, and have advantages such as cost is low, clean and safe.
According to wurtzite CuInS provided by the invention 2The preparation method of nanometer plate is because add complexing agent (HOCH 2CH 2) 3Behind the N, synthetic wurtzite CuInS 2Nanometer plate is along with its XRD crest of increase in reaction times changes and translation significantly, so it has good stability, phase purity is very high and do not find other dephasigns.So, wurtzite CuInS 2Nanometer plate can stably exist at ambient temperature and can not change yellow copper structure into.The wurtzite CuInS that this method realizes 2Nanometer plate stability is high and have a tunable nanometer energy level of broadband.Simultaneously, this wurtzite CuInS 2Nanometer plate UV rational curve has greatly improved, and it absorbs sideband and becomes more obvious, can the band value be about 1.45 eV through estimating it.
Description of drawings
Fig. 1 is the present invention synthetic Wurzite structure CuInS in an embodiment 2The Wurzite structure CuInS of nanometer plate and differential responses time contract 2X ray diffraction (XRD) collection of illustrative plates of nanometer plate;
Fig. 2 is that the reaction times is 150 min synthetic Wurzite structure CuInS in an embodiment in the present invention 2Nanometer plate is amplified 1*10 5The FE-SEM figure of multiplying power;
Fig. 3 is that the reaction times is 150 min synthetic Wurzite structure CuInS in an embodiment in the present invention 2Nanometer plate is amplified 2*10 4The FE-SEM figure of multiplying power;
Fig. 4 is the present invention synthetic Wurzite structure CuInS in an embodiment 2The Wurzite structure CuInS of nanometer plate and differential responses time contract 2The UV absorption spectrum curve of nanometer plate.
Embodiment
The invention will be further described below in conjunction with accompanying drawing and specific embodiment.
The Wurzite structure CuInS of present embodiment 2The synthetic method of nanometer plate may further comprise the steps:
Steps A:
Pack in the round-bottomed flask of the 100 mL capacity glycol ether of 40 mL, the glycol ether chemical formula is HO-CH 2-CH 2-O-CH 2-CH 2-OH, English diethylene glycol by name.Again with the CuCl of 1 mmol 2.2H 2The InCl of O and 1 mmol 3.4H 2O mixes the diethylene glycol solution that adds in the round-bottomed flask.The round-bottomed flask that fills solution is positioned in the heating unit heats, and its speed with 550 rpms is carried out magnetic agitation, up to CuCl 2.2H 2O and InCl 3.4H 2O fully is dissolved in diethylene glycol solution.The color of solution gradually become yellow by initial bright yellow-green colour and color thin out gradually until light yellow.
Simultaneously, with the thiocarbamide of 4 mmol, the chemical formula of thiocarbamide is SC (NH 2) 2, English thiourea by name adds 20 mL glycol ethers.Stir at ambient temperature up to thiocarbamide and fully be dissolved in diethylene glycol solution.
Step B:
To contain CuCl 2.2H 2O and InCl 3.4H 2It vacuumizes the solution of O and handles 30 min, exhausts logical about 5 min of nitrogen after the vacuum; Carry out once the processing that vacuumizes of about 10 min again, and then logical nitrogen.And begin containing CuCl 2.2H 2O and InCl 3.4H 2The solution of O heats, and treats that solution temperature progressively is raised to 180 oDuring C, add the trolamine liquid of 3mL earlier, the chemical formula of trolamine is (HOCH 2CH 2) 3N, English triethanolamine by name.Add and to present flaxen liquid color behind the trolamine originally and add gradually and be deep to brownly, but this mixing solutions is still clear and do not have any precipitation and occur.The solution that will contain thiocarbamide again is injected in the blended solution.
Step C:
To contain CuCl 2.2H 2O and InCl 3.4H 2The mixing solutions of O, trolamine and thiocarbamide is 180 oReacting by heating 150min in the C nitrogen environment.Reaction naturally cools to room temperature with it after finishing.
Step D:
The mixing liquid that cools off the back gained is separated drying, may further comprise the steps:
The mixing liquid of cooling back gained is added an amount of alcohol and separates 5 min with 8000 rpms speed with whizzer.After separating through whizzer, black precipitate will be stayed the centrifuge tube bottom, waste collection and handle; In above-mentioned black precipitate, add alcohol and separate once more, outwell the gained supernatant liquor, collect the gained black precipitate; Said process is repeated 3 ~ 5 times, add an amount of alcohol thorough mixing in the gained precipitation, this mixing solutions is placed loft drier, dry several hrs obtains black powder under 80 ℃ temperature condition, i.e. Wurzite structure CuInS 2Nanometer plate.
The Wurzite structure CuInS of present embodiment 2The reaction times of the synthetic method of nanometer plate is 150 min.Also having done the reaction times in addition is decided to be 30 min, 60 min, 90 min, 120 min, 180 min and 240 min respectively, and other operation stepss are identical, synthesized different Wurzite structure CuInS of reaction times 2Nanometer plate.
Fig. 1 is the present invention synthetic Wurzite structure CuInS in an embodiment 2The Wurzite structure CuInS of nanometer plate and differential responses time contract 2X ray diffraction (XRD) collection of illustrative plates of nanometer plate.
As shown in Figure 1, wherein, the phase place of this material of numeral in the bracket, a, b, c, d, e, f, g represent that respectively the time of building-up reactions is the product of 30 min, 60 min, 90 min, 120 min, 150 min, 180 min, 240 min.From Fig. 1, can be observed, increase along with the time, the peak value of institute's synthetic product is skew or change significantly not, illustrate that institute's synthetic material is more stable, but also as can be seen when the reaction times is 150 min, the obvious more and half-peak width increase of the peak value of institute's synthetic product, crystalline structure is better.This illustrates that this reaction times is relatively more suitable, is chosen as optimum generated time.Can contrast from Fig. 1, each peak value of this material may be defined as (1 0 0), (0 0 2), (1 0 1), (1 0 2), (1 1 0), (1 0 3), (1 1 2).This peak value and document (by Bonil Koo, Reken N. Patel and Brian A. Korgel are delivered) " Wurtzite-Chalcopyrite Polytypism in CuInS 2Nanodisks " CuInS of the Wurzite structure reported 2Peak value is very consistent, and preparation method's synthetic material of the present invention is the CuInS with Wurzite structure 2In addition, this synthetic schemes institute synthetic material stability is very high as can be seen, and does not have other dephasigns to occur, and has shown superior performance.
Fig. 2 is the present invention synthetic Wurzite structure CuInS in an embodiment 2Nanometer plate is amplified 1*10 5The FE-SEM figure of multiplying power.
Fig. 3 is the present invention synthetic Wurzite structure CuInS in an embodiment 2Nanometer plate is amplified 2*10 4The FE-SEM figure of multiplying power.
As shown in Figures 2 and 3, determine that by Fig. 1 the synthetic product presents the CuInS of Wurzite structure 2, further can know that by Fig. 2 and Fig. 3 this material is discous, obtain Wurzite structure CuInS according to magnification 2The minimum diameter of nanometer plate is about 100 nm, and thickness is about 10 nm.
Fig. 4 is the present invention synthetic Wurzite structure CuInS in an embodiment 2The Wurzite structure CuInS of nanometer plate and differential responses time contract 2The UV absorption spectrum curve of nanometer plate.
As shown in Figure 4, by adding complexing agent (HOCH 2CH 2) 3After the N, the wurtzite CuInS that obtains 2The UV of nanometer plate absorbs sideband and becomes very precipitous and obvious.Reaction times is 30 min, 60 min, 90 min, 120 min, 150 min, the Wurzite structure CuInS that 180 min and 240 min obtain 2The energy band value of nanometer plate be followed successively by 1.50 eV, 1.439 eV, 1.480 eV, 1.447 eV, 1.468 eV, 1.42 eV and 1.442 eV.1.45 eV are very approaching with the desirable energy of solar cell band value.So it has shown good photovoltaic property.Reaction times is that 150 min prepare synthetic Wurzite structure CuInS 2The energy band value of nanometer plate is the most near desirable 1.45 eV.
The effect of embodiment and effect
The wurtzite CuInS that provides according to present embodiment 2The preparation method of nanometer plate is a kind of gentleness relatively and the solvent of environmental protection because solvent uses glycol ether, and it has colourless, odorless, transparent, hygroscopic thick liquid, pungent sweet taste is arranged, non-corrosiveness, low toxicity.245 ℃ of boiling points, fusing point-6.5 ℃, zero pour-10.45 ℃, flash-point 123.9, specific refractory power 1.4472, relative density 1.1184, viscosity 0.30 pool, so other polar solvents such as soluble in water, pure, acetone, ether, ethylene glycol are its excellent property; And glycol ether is compared with oleyl amine, and its price is also relatively cheap.So, can realize preparation wurtzite CuInS under 180 ℃ of conditions of lower temperature 2Nanometer plate, and have advantages such as cost is low, clean and safe.
According to wurtzite CuInS provided by the invention 2The preparation method of nanometer plate is because add complexing agent (HOCH 2CH 2) 3Behind the N, synthetic wurtzite CuInS 2Nanometer plate is along with its XRD crest of increase in reaction times changes and translation significantly, so it has good stability, phase purity is very high and do not find other dephasigns.So, wurtzite CuInS 2Nanometer plate can stably exist at ambient temperature and can not change yellow copper structure into.The wurtzite CuInS that this method realizes 2Nanometer plate stability is high and have a tunable nanometer energy level of broadband.
According to wurtzite CuInS provided by the invention 2The preparation method of nanometer plate is because the wurtzite CuInS that the reaction times is 150 min to be obtained 2The obvious more and half-peak width increase of peak value that nanometer plate obtains through the X ray diffraction, so, wurtzite CuInS 2The crystalline structure of nanometer plate is better.

Claims (5)

1. wurtzite CuInS 2The preparation method of nanometer plate is characterized in that, may further comprise the steps:
A. with CuCl 22H 2O and InCl 34H 2O fully is dissolved in glycol ether and obtains solution one, with SC (NH 2) 2Fully be dissolved in glycol ether and obtain solution two;
B. described solution one is heated to 180 ℃ in the anhydrous and oxygen-free environment, adds (HOCH earlier 2CH 2) 3N liquid mixes obtaining solution three again with described solution two;
C. described solution three reacts under 180 ℃ of temperature and protection of nitrogen gas, and the reaction times is 30～240min, naturally cools to room temperature after reaction finishes and obtains mixing solutions;
D. described mixing solutions is separated drying, obtain described Wurzite structure CuInS2 nanometer plate;
Wherein, described CuCl 2.2H 2O amount of substance: InCl 3.4H 2O amount of substance: SC (NH 2) 2Amount of substance: (HOCH 2CH 2) 3The ratio of N volume is 1mol:1mol:4mol:3L.
2. wurtzite CuInS according to claim 1 2The preparation method of nanometer plate is characterized in that:
Wherein, fully carry out magnetic agitation in the dissolved process described in the steps A.
3. wurtzite CuInS according to claim 1 2The preparation method of nanometer plate is characterized in that:
Wherein, anhydrous and oxygen-free environment described in the step B is to realize by alternately vacuumizing and feed nitrogen.
4. wurtzite CuInS according to claim 1 2The preparation method of nanometer plate is characterized in that:
Wherein, the reaction times described in the step C is 150 min.
5. wurtzite CuInS according to claim 1 2The preparation method of nanometer plate is characterized in that:
Wherein, separating exsiccant described in the step D may further comprise the steps:
D1. after in described mixing solutions, adding alcohol, separate acquisition initial precipitation thing with whizzer;
D2. after in described initial precipitation thing, adding alcohol, separate the acquisition throw out with whizzer;
D3. repeating step D2 is three to five times, obtains final throw out;
D4. after in described final throw out, adding alcohol, in loft drier, carry out drying, obtain described Wurzite structure CuInS 2Nanometer plate.
CN2013101461975A 2013-04-25 2013-04-25 Preparation method of wurtzite CuInS2 nanodisk Pending CN103214029A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103496737A (en) * 2013-09-26 2014-01-08 南京师范大学 Method for synthesizing copper-indium sulfide quantum dot in one step through microwave process
CN107059131A (en) * 2017-04-21 2017-08-18 南京信息工程大学 A kind of semiconductor nano and preparation method and application
CN111977685A (en) * 2020-06-09 2020-11-24 河南大学 Preparation method of sodium ion battery negative electrode material

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CN102887538A (en) * 2012-10-15 2013-01-23 江苏科技大学 Preparation method of surfactant-modified CuInS2 nanocrystal

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CN102887538A (en) * 2012-10-15 2013-01-23 江苏科技大学 Preparation method of surfactant-modified CuInS2 nanocrystal

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103496737A (en) * 2013-09-26 2014-01-08 南京师范大学 Method for synthesizing copper-indium sulfide quantum dot in one step through microwave process
CN107059131A (en) * 2017-04-21 2017-08-18 南京信息工程大学 A kind of semiconductor nano and preparation method and application
CN111977685A (en) * 2020-06-09 2020-11-24 河南大学 Preparation method of sodium ion battery negative electrode material
CN111977685B (en) * 2020-06-09 2022-09-02 河南大学 Preparation method of sodium ion battery negative electrode material

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Application publication date: 20130724