CN104057101B - The method of copper indium tellurium nano-wire is prepared in a kind of catalysis - Google Patents
The method of copper indium tellurium nano-wire is prepared in a kind of catalysis Download PDFInfo
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Abstract
The method of copper indium tellurium nano-wire is prepared in a kind of catalysis; belong to thin-film solar cells manufacture of materials technical field of new generation; first prepare the toluene solution of bismuth nanoparticle and the precursor solution containing indium acetate, cuprous acetate and tellurium respectively; again under nitrogen protection; after tri octyl phosphine is heated; add the toluene solution of bismuth nanoparticle; drip the precursor solution containing indium acetate, cuprous acetate and tellurium again; after question response terminates; through cooling the toluene that reinjects; then centrifugal, get solid phase toluene centrifuge washing final vacuum dry, obtain copper indium tellurium nano-wire.The present invention is with metal bismuth nanoparticle for catalyst, and the instrument and equipment of employing is cheap, and operating process is easy, effectively can control the stoichiometric proportion of multi-component material, obtains highly purified copper indium tellurium nano-wire, can the high-quality nano wire of large batch of production.In addition, by regulating the concentration of bismuth nanoparticle, or the concentration of presoma can regulate and control the length of nano wire.
Description
Technical field
The invention belongs to thin-film solar cells manufacture of materials technical field of new generation, be specifically related to the method preparing copper indium tellurium nano-wire.
Background technology
The preparation method of one dimension semiconductor nano wire is mainly divided into vapor phase method and liquid phase method, wherein vapor phase method needs instrument and equipment costly, operating process is comparatively complicated, comparatively serious to wastage of material, can not effectively control multi-component stoichiometric proportion, the nano wire limits throughput synthesized, these all limit practical application prepared by material.Compared with vapor phase method, especially Solution-Liquid-Solid(SLS) to have instrument and equipment cheap for method, and operating process is easy, effectively can control the stoichiometric proportion of multi-component material, can the high-quality nano wire of large batch of production, meet commercialization needs.SLS side's ratio juris is with the metal nanoparticle of low melting point for catalyst (as: tin, bismuth), and at high temperature metal nanoparticle is assembled for liquid droplet, and these drops are using the liquid core as nanowire growth.Reaction precursor cognition constantly dissolves in liquid droplet, and when reaching supersaturation, semiconductor dendrite arm will be separated out from drop, under the constraint of drop, forms 1-dimention nano line structure.Precursor concentration undersaturation in drop simultaneously, presoma can dissolve in drop, provides dendrite arm continued growth, and the nano wire formed like this can reach 10 microns.
CIS (CuInSe
2, CIS) and be a kind of I-III-VI compound semiconductor, there are chalcopyrite, zincblende two allotropic crystal structures.Copper, indium and selenium film solar cell material has the optical energy gap of near optimal, absorptivity (absorbing the ratio with incident flux) high (10
5cm
– 1), the features such as the strong and long-time stability of capability of resistance to radiation are good.Its energy gap can also replace In by Ga and Al part, or S part replacement Se regulates.Copper, indium and selenium film solar cell belongs to the very high compound semiconductor light volt device of Integration ofTechnology degree, is made up of the deposited on substrates plural layers at glass or cheapness.Overall film thickness about 2 ~ 3 μm, has the combination properties such as high conversion efficiency, low cost, nothing decline.Germany, the U.S. and Japan have completed copper, indium and selenium film solar cell Semi-plant scale, start to enter the tackling key problem of extensive industrialization technology.Showa oil company of Japan has created the highest world record of this CIS series film solar battery conversion efficiency.Area is 864cm
2conversion efficiency be 14.3%, area is 3560cm
2conversion efficiency be 13.4%.
Copper indium tellurium (CuInTe
2, CIT) be also a kind of I-III-VI compound semiconductor, its energy gap is 1.02eV, close with CIS, has good photo absorption performance, is a kind of potential thin-film solar cells material.Have been reported and synthesized copper indium tellurium nano particle by microwave irradiation, solvent-thermal method etc., but there is not been reported about the preparation method of copper indium tellurium nano-wire.
Summary of the invention
The object of the invention is to the catalysis preparation method proposing a kind of thin-film solar cells material-copper indium tellurium nano-wire.
The present invention includes following steps:
1) toluene solution of bismuth nanoparticle is prepared:
The tetrahydrofuran solution of two (trimethyl silicon based) amino bismuth is mixed with the tetrahydrofuran solution of pair (trimethyl silicon based) Sodamide, forms the mixed solution containing bismuth presoma;
Under nitrogen protection, by polyvinylpyrrolidone-hexadecane block copolymer and diphenyl ether mixing, magnetic agitation is also heated to 180 DEG C, forming reactions system;
Mixed solution containing bismuth presoma is injected reaction system, after reacting 30 minutes, cool to room temperature, centrifugal after adding methyl alcohol again, by toluene and methyl alcohol dispersion and centrifugal treating, by centrifugal go out solid phase dispersion in toluene, form the toluene solution of bismuth nanoparticle;
2) precursor solution of preparation containing indium acetate, cuprous acetate and tellurium:
Under nitrogen protection tellurium powder is dissolved in tri octyl phosphine, forms the tri octyl phosphine solution that tellurium content is the tellurium of 0.5 ~ 1mol/L;
The present invention selects tri octyl phosphine to have three advantages as solvent: 1. tri octyl phosphine is a high boiling organic solvent, and the present invention needs higher reaction temperature, and tri octyl phosphine can be satisfied the demand; 2. tri octyl phosphine can well dissolve various presoma; 3. tri octyl phosphine has certain reproducibility, can protective reaction thing not oxidized.
Under oxygen free condition, after indium acetate, cuprous acetate, oleic acid and tri octyl phosphine being mixed, add the tri octyl phosphine solution of tellurium, form the precursor solution containing indium acetate, cuprous acetate and tellurium;
3) copper indium tellurium nano-wire is prepared:
Under nitrogen protection; tri octyl phosphine is heated to 360 ~ 370 DEG C; under heat-retaining condition; add the toluene solution of bismuth nanoparticle, then drip the precursor solution containing indium acetate, cuprous acetate and tellurium, after question response terminates; through cooling the toluene that reinjects; then centrifugal, get solid phase toluene centrifuge washing final vacuum dry, obtain copper indium tellurium nano-wire.
According to reaction principle, reaction temperature must higher than the fusing point of bismuth metal, namely more than 273.1 DEG C, and bismuth nanoparticle is liquid phase in reaction system, and presoma can be dissolved in bismuth nanoparticle, grows dendrite arm line after supersaturation.But for the synthesis of copper indium tellurium nano-wire, when lower than 360 DEG C, due to the reactivity that it is high, copper indium tellurium can automatic nucleation, form nanometer spherical copper indium tellurium.As temperature higher than 370 DEG C time, tri octyl phosphine start backflow.Therefore the present invention's first tri octyl phosphine in step 3) is heated to 360 ~ 370 DEG C, and under heat-retaining condition, adds the toluene solution of bismuth nanoparticle.
The present invention is with metal bismuth nanoparticle for catalyst, and adopt the advantage of the toluene solution of bismuth nanoparticle to be the concentration that effectively can control bismuth nanoparticle on the one hand, liquid form can facilitate taking of catalyst on the other hand.
The advantage of the above processing step of the present invention is: the instrument and equipment of employing is cheap, and operating process is easy, effectively can control the stoichiometric proportion of multi-component material, obtains highly purified copper indium tellurium nano-wire, can the high-quality nano wire of large batch of production.In addition, by regulating the concentration of bismuth nanoparticle, or the concentration of presoma can regulate and control the length of nano wire.
In described step 3), in the toluene solution of described bismuth nanoparticle, the sub-concentration of bismuth nanoparticle is 5 ~ 20mg/mL.Concentration as sub-in bismuth nanoparticle is lower than 5mg/mL, and reactant meeting spontaneous nucleation, can not form nano wire; Concentration as sub-in bismuth nanoparticle is higher than 20mg/mL, and the concentration of reactant presoma in liquid bismuth nanoparticle is too low, can not reach supersaturation, generates dendrite arm and nano wire.So the sub-concentration of bismuth nanoparticle 5 ~ 20mg/mL is the most suitable.
In order to realize bismuth nanoparticle toluene solution in the sub-concentration of bismuth nanoparticle be 5 ~ 20mg/mL, concrete grammar is: in step 1), for the preparation of two (trimethyl silicon based) the amino bi concns in the tetrahydrofuran solution of described two (trimethyl silicon based) amino bismuth of the mixed solution containing bismuth presoma for there being 1mol/L, two (trimethyl silicon based) Sodamide concentration in the tetrahydrofuran solution of described two (trimethyl silicon based) Sodamide are 1mol/L, the tetrahydrofuran solution of described two (trimethyl silicon based) amino bismuth is 1 ︰ 4 with the mixed material feeding volume ratio of the tetrahydrofuran solution of two (trimethyl silicon based) Sodamide.This volume ratio, mainly in order to control the speed that bismuth is reduced, obtains bismuth nanoparticle of size tunable.
In step 1), be 1 ︰ 3 for the preparation of the polyvinylpyrrolidone-hexadecane block copolymer of reaction system and the mixing quality ratio of diphenyl ether.This ratio can ensure that polyvinylpyrrolidone-hexadecane block copolymer can be dissolved completely in diphenyl ether, and maintains block copolymer concentration suitable in reaction system.
In step 1), described two tetrahydrofuran solution of (trimethyl silicon based) amino bismuth and the mixing ratio of polyvinylpyrrolidone-hexadecane block copolymer are 0.5mL ︰ 5g.This volume ratio can obtain suitable reactant concentration, obtains the nano particle of size tunable.
Described step 2) in, in a nitrogen atmosphere, indium acetate, cuprous acetate, oleic acid and tri octyl phosphine mixed through magnetic agitation and is heated to 90 ~ 110 DEG C, through insulation deoxygenation, then after being cooled to normal temperature, adding the tri octyl phosphine solution of tellurium.Mix and blend at 90 ~ 110 DEG C, is mainly dissolved in tri octyl phosphine by indium acetate and cuprous acetate, and at this temperature, indium acetate, cuprous acetate, oleic acid and tri octyl phosphine can not react, and can form transparent solution.
Described step 2) in, the mixing mol ratio of indium acetate, cuprous acetate and tellurium is 1 ︰ 1 ︰ 2.This feeds intake according to the stoichiometric proportion of compound, ensures the purity of product.
In order to ensure the concentration that each reactant keeps suitable in reaction system, obtain purity, degree of crystallinity good copper indium tellurium nano-wire, in described step 3), the toluene solution of described tri octyl phosphine, described bismuth nanoparticle and the volume ratio that feeds intake of the described precursor solution containing indium acetate, cuprous acetate and tellurium are 10 ︰ 0.1 ~ 0.5 ︰ 4 ~ 10.
In described step 3), described vacuum drying temperature conditions is 50 DEG C, vacuum is-0.1MPa ~-0.3MPa.Can ensure that dry run does not have Oxygen Adsorption at material surface, avoid it to affect the opto-electronic conversion performance of material.
Accompanying drawing explanation
Fig. 1,2 is respectively the transmission electron microscope picture of the copper indium tellurium nano-wire of preparation.
Fig. 3 is the scanning electron microscope (SEM) photograph of the copper indium tellurium nano-wire of preparation.
Fig. 4 is the X-ray powder diffraction pattern of the copper indium tellurium nano-wire of preparation.
Fig. 5 is the distribution diagram of element of the copper indium tellurium nano-wire of preparation.
Fig. 6 is the VA characteristic curve that the copper indium tellurium nano-wire made in the process of the present invention is assembled into thin-film solar cells.
Detailed description of the invention
One, in order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is described in detail.
Embodiment one:
1, Kaolinite Preparation of Catalyst---the toluene solution of bismuth nanoparticle:
The tetrahydrofuran solution of two (trimethyl silicon based) the amino bismuth of the 1mol/L being by 0.5mL, two (trimethyl silicon based) amino bi content and 2mL, two (trimethyl silicon based) Sodamide content are the tetrahydrofuran solution mixing of two (trimethyl silicon based) Sodamides of 1mol/L, form the mixed solution containing bismuth presoma, and be placed in syringe.
Separately get 5g polyvinylpyrrolidone-hexadecane block copolymer and 15g diphenyl ether under nitrogen protection, magnetic agitation is also heated to 180 DEG C, forming reactions system.
Be expelled in reaction system by the mixed solution containing bismuth presoma, the rapid variable color of solution, becomes black.After reacting 30 minutes, remove thermal source, after cool to room temperature, centrifugal after adding 30mL methyl alcohol again, with the mixed solvent repetitive cycling of toluene and methyl alcohol carry out disperseing, after centrifugally operated 3 ~ 4 times, solids product after centrifugal is for the last time dispersed in toluene, forms the toluene solution of bismuth nanoparticle.
After tested, in the toluene solution of bismuth nanoparticle, the concentration of bismuth nanoparticle is 5mg/mL.Adopt the test of transmission electron microscope method, the diameter of bismuth nanoparticle is 15 ± 1nm.
2, preparation feedback presoma:
Take solid tellurium powder 2.55g, under nitrogen protection, it be all dissolved in 20mL tri octyl phosphine, forming tellurium concentration in the precursor solution of tellurium is 1mol/L.
0.5mmol (0.145g) indium acetate, 0.5mmol (0.06g) cuprous acetate, 0.5mL oleic acid and 8mL tri octyl phosphine are mixed, in a nitrogen atmosphere magnetic agitation heating, temperature maintains 110 DEG C, the abundant deoxygenation through 30 minutes.Then, remove thermal source, by mixed system cool to room temperature, the precursor solution getting 1mL tellurium joins in above-mentioned mixed solution, after fully stirring, as precursors---the precursor solution containing indium acetate, cuprous acetate and tellurium.
3, copper indium tellurium nano-wire is prepared:
Under nitrogen protection, by 10mL tri octyl phosphine in vessel in heating to 370 DEG C.Then, the toluene solution getting 0.5mL bismuth nanoparticle is expelled in tri octyl phosphine rapidly, then dropping 9.5mL is contained the precursor solution of indium acetate, cuprous acetate and tellurium, keeps system temperature within the scope of 365 ~ 370 DEG C.
After dropwising, then react 5 minutes, remove the thermal source outside container, make reacted system be cooled to 70 DEG C.
In system, inject 10mL toluene again, then centrifugal, then use toluene cyclic washing product, obtain solid phase 50 DEG C, vacuum is dry under being the condition of-0.1MPa, obtains copper indium tellurium nano-wire.
Embodiment 2
1, Kaolinite Preparation of Catalyst---the toluene solution of bismuth nanoparticle:
The tetrahydrofuran solution of two (trimethyl silicon based) the amino bismuth of the 1mol/L being by 0.5mL, two (trimethyl silicon based) amino bi content and 2mL, two (trimethyl silicon based) Sodamide content are the tetrahydrofuran solution mixing of two (trimethyl silicon based) Sodamides of 1mol/L, form the mixed solution containing bismuth presoma, and be placed in syringe.
Separately get 5g polyvinylpyrrolidone-hexadecane block copolymer and 15g diphenyl ether under nitrogen protection, magnetic agitation is also heated to 180 DEG C, forming reactions system.
Be expelled in reaction system by the mixed solution containing bismuth presoma, the rapid variable color of solution, becomes black.After reacting 30 minutes, remove thermal source, after cool to room temperature, centrifugal after adding 30mL methyl alcohol again, with the mixed solvent repetitive cycling of toluene and methyl alcohol carry out disperseing, after centrifugally operated 3 ~ 4 times, the product after centrifugal be for the last time dispersed in toluene, form the toluene solution of bismuth nanoparticle.
After tested, in the toluene solution of bismuth nanoparticle, the concentration of bismuth nanoparticle is 10mg/mL.Adopt the test of transmission electron microscope method, the diameter of bismuth nanoparticle is 15 ± 1nm.
2, preparation feedback presoma:
Take solid tellurium powder 2.55g, under nitrogen protection, it be all dissolved in 20mL tri octyl phosphine, forming tellurium concentration in the precursor solution of tellurium is 1mol/L.
0.25mmol (0.073g) indium acetate, 0.25mmol (0.03g) cuprous acetate, 0.25mL oleic acid and 4mL tri octyl phosphine are mixed, in a nitrogen atmosphere magnetic agitation heating, temperature maintains 110 DEG C, the abundant deoxygenation through 30 minutes.Then, remove thermal source, by mixed system cool to room temperature, the precursor solution getting 0.5mL tellurium joins in above-mentioned mixed solution, after fully stirring, as precursors---the precursor solution containing indium acetate, cuprous acetate and tellurium.
3, copper indium tellurium nano-wire is prepared:
Under nitrogen protection, by 10mL tri octyl phosphine in vessel in heating to 365 DEG C.Then, the toluene solution getting 0.25mL bismuth nanoparticle is expelled in tri octyl phosphine rapidly, then dropping 4.75mL is contained the precursor solution of indium acetate, cuprous acetate and tellurium, keeps system temperature within the scope of 365 ~ 370 DEG C.
After dropwising, then react 6 minutes, remove the thermal source outside container, make reacted system be cooled to 70 DEG C.
In system, inject 10mL toluene again, then centrifugal, then use toluene cyclic washing product, obtain solid phase 50 DEG C, vacuum is dry under being the condition of-0.2MPa, obtains copper indium tellurium nano-wire.
Embodiment 3
1, Kaolinite Preparation of Catalyst---the toluene solution of bismuth nanoparticle:
The tetrahydrofuran solution of two (trimethyl silicon based) the amino bismuth of the 1mol/L being by 0.5mL, two (trimethyl silicon based) amino bi content and 2mL, two (trimethyl silicon based) Sodamide content are the tetrahydrofuran solution mixing of two (trimethyl silicon based) Sodamides of 1mol/L, form the mixed solution containing bismuth presoma, and be placed in syringe.
Separately get 5g polyvinylpyrrolidone-hexadecane block copolymer and 15g diphenyl ether under nitrogen protection, magnetic agitation is also heated to 180 DEG C, forming reactions system.
Be expelled in reaction system by the mixed solution containing bismuth presoma, the rapid variable color of solution, becomes black.After reacting 30 minutes, remove thermal source, after cool to room temperature, centrifugal after adding 30mL methyl alcohol again, with the mixed solvent repetitive cycling of toluene and methyl alcohol carry out disperseing, after centrifugally operated 3 ~ 4 times, the product after centrifugal be for the last time dispersed in toluene, form the toluene solution of bismuth nanoparticle.
After tested, in the toluene solution of bismuth nanoparticle, the concentration of bismuth nanoparticle is 20mg/mL.Adopt the test of transmission electron microscope method, the diameter of bismuth nanoparticle is 15 ± 1nm.
2, preparation feedback presoma:
Take solid tellurium powder 1.28g, under nitrogen protection, it be all dissolved in 20mL tri octyl phosphine, forming tellurium concentration in the precursor solution of tellurium is 0.5mol/L.
0.5mmol (0.145g) indium acetate, 0.5mmol (0.06g) cuprous acetate, 0.5mL oleic acid and 6mL tri octyl phosphine are mixed, in a nitrogen atmosphere magnetic agitation heating, temperature maintains 110 DEG C, the abundant deoxygenation through 30 minutes.Then, remove thermal source, by mixed system cool to room temperature, the precursor solution getting 2mL tellurium joins in above-mentioned mixed solution, after fully stirring, as precursors---the precursor solution containing indium acetate, cuprous acetate and tellurium.
3, copper indium tellurium nano-wire is prepared:
Under nitrogen protection, by 10mL tri octyl phosphine in vessel in heating to 370 DEG C.Then, the toluene solution getting 0.1mL bismuth nanoparticle is expelled in tri octyl phosphine rapidly, then dropping 8.5mL is contained the precursor solution of indium acetate, cuprous acetate and tellurium, keeps system temperature within the scope of 365 ~ 370 DEG C.
After dropwising, then react 7 minutes, remove the thermal source outside container, make reacted system be cooled to 70 DEG C.
In system, inject 11mL toluene again, then centrifugal, then use toluene cyclic washing product, obtain solid phase 50 DEG C, vacuum is dry under being the condition of-0.3MPa, obtains copper indium tellurium nano-wire.
Two, product checking:
As shown in Figure 1, 2, the difference of copper indium tellurium nano-wire for adopting the inventive method to prepare amplify accompany several under transmission electron microscope picture.Visible: prepared product is nano wire, length is at some tens of pm, and diameter is at 100 ran.
As shown in Figure 3, the scanning electron microscope (SEM) photograph of copper indium tellurium nano-wire for adopting the inventive method to prepare.Visible, prepared product is nano wire.
Fig. 4 is the X-ray powder diffraction pattern of the copper indium tellurium nano-wire adopting the inventive method to prepare.Visible: prepared sample is pure copper indium tellurium (CuInTe
2), not miscellaneous containing other.The vertical line being wherein arranged in below is the characteristic diffraction peak position of standard spectrogram.
Fig. 5 is the distribution diagram of element of the copper indium tellurium nano-wire adopting the inventive method to prepare.Visible, nano wire consist of copper, indium, tellurium, the atomic ratio of three is 1:1:2.
Three, the effect in thin-film solar cells manufacture of materials:
Fig. 6 shows the VA characteristic curve after adopting the copper indium tellurium nano-wire prepared of the inventive method to be assembled into thin-film solar cells.
As shown in Figure 6, curve a represents VA characteristic curve during solar cell applying bias in complete dark situation, and curve b represents constant light according to VA characteristic curve during lower solar cell no-bias.As can be seen from Fig. 6, copper indium tellurium nano-wire prepared by utilization is assembled into thin-film solar cells, this battery has photoelectric respone after testing, photoelectric transformation efficiency is 1.226%, open-circuit voltage is 0.37V, illustrate that copper indium tellurium nano-wire as photoelectric conversion material, can be applied to thin-film solar cells, there is certain potential using value.By the improvement of battery preparation technique, the photoelectric transformation efficiency of battery can be improved further.
Claims (9)
1. a method for copper indium tellurium nano-wire is prepared in catalysis, it is characterized in that comprising the following steps:
1) toluene solution of bismuth nanoparticle is prepared:
The tetrahydrofuran solution of two (trimethyl silicon based) amino bismuth is mixed with the tetrahydrofuran solution of pair (trimethyl silicon based) Sodamide, forms the mixed solution containing bismuth presoma;
Under nitrogen protection, by polyvinylpyrrolidone-hexadecane block copolymer and diphenyl ether mixing, magnetic agitation is also heated to 180 DEG C, forming reactions system;
Mixed solution containing bismuth presoma is injected reaction system, after reacting 30 minutes, cool to room temperature, centrifugal after adding methyl alcohol again, by mixed solvent dispersion and the centrifugal treating of toluene and methyl alcohol, by centrifugal go out solid phase dispersion in toluene, form the toluene solution of bismuth nanoparticle;
2) precursor solution of preparation containing indium acetate, cuprous acetate and tellurium:
Under nitrogen protection tellurium powder is dissolved in tri octyl phosphine, forms the tri octyl phosphine solution that tellurium content is the tellurium of 0.5 ~ 1mol/L; Under oxygen free condition, after indium acetate, cuprous acetate, oleic acid and tri octyl phosphine being mixed, add the tri octyl phosphine solution of tellurium, form the precursor solution containing indium acetate, cuprous acetate and tellurium;
3) copper indium tellurium nano-wire is prepared:
Under nitrogen protection; tri octyl phosphine is heated to 360 ~ 370 DEG C; under heat-retaining condition; add the toluene solution of bismuth nanoparticle, then drip the precursor solution containing indium acetate, cuprous acetate and tellurium, after question response terminates; through cooling the toluene that reinjects; then centrifugal, get solid phase toluene centrifuge washing final vacuum dry, obtain copper indium tellurium nano-wire.
2. preparation method according to claim 1, is characterized in that in described step 3), and in the toluene solution of described bismuth nanoparticle, the sub-concentration of bismuth nanoparticle is 5 ~ 20mg/mL.
3. preparation method according to claim 1 and 2, it is characterized in that in step 1), be 1mol/L for the preparation of two (trimethyl silicon based) the amino bi concns in the tetrahydrofuran solution of described two (trimethyl silicon based) amino bismuth of the mixed solution containing bismuth presoma, two (trimethyl silicon based) Sodamide concentration in the tetrahydrofuran solution of described two (trimethyl silicon based) Sodamide are 1mol/L, and the tetrahydrofuran solution of described two (trimethyl silicon based) amino bismuth is 1 ︰ 4 with the mixed material feeding volume ratio of the tetrahydrofuran solution of two (trimethyl silicon based) Sodamide.
4. preparation method according to claim 3, is characterized in that in step 1), is 1 ︰ 3 for the preparation of the polyvinylpyrrolidone-hexadecane block copolymer of reaction system and the mixing quality ratio of diphenyl ether.
5. preparation method according to claim 4, is characterized in that in step 1), and described two tetrahydrofuran solution of (trimethyl silicon based) amino bismuth and the mixing ratio of polyvinylpyrrolidone-hexadecane block copolymer are 0.5mL ︰ 5g.
6. preparation method according to claim 1, it is characterized in that described step 2) in, in a nitrogen atmosphere, indium acetate, cuprous acetate, oleic acid and tri octyl phosphine are mixed through magnetic agitation and is heated to 90 ~ 110 DEG C, through insulation deoxygenation, then after being cooled to normal temperature, add the tri octyl phosphine solution of tellurium.
7. preparation method according to claim 6, is characterized in that described step 2) in, the mixing mol ratio of indium acetate, cuprous acetate and tellurium is 1 ︰ 1 ︰ 2.
8. preparation method according to claim 1, it is characterized in that in described step 3), the toluene solution of described tri octyl phosphine, described bismuth nanoparticle and the volume ratio that feeds intake of the described precursor solution containing indium acetate, cuprous acetate and tellurium are 10 ︰ 0.1 ~ 0.5 ︰ 4 ~ 10.
9. preparation method according to claim 1, is characterized in that in described step 3), and described vacuum drying temperature conditions is 50 DEG C, vacuum is-0.1MPa ~-0.3MPa.
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| JPH01298011A (en) * | 1988-05-26 | 1989-12-01 | Mitsubishi Metal Corp | Production of metal telluride |
| CN101700871A (en) * | 2009-10-26 | 2010-05-05 | 中国科学技术大学 | Copper-indium-selenium nanowire array and preparation method and application thereof |
| CN102208487A (en) * | 2011-04-22 | 2011-10-05 | 西安交通大学 | Preparation method of nanostructure heterojunction of CuInSe nanocrystal, cadmium sulfide quantum dot and zinc oxide nanowire array |
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