CN102790129B - Manufacturing method for core-shell structure CdSe/CdS nanocrystalline for photovoltaic device - Google Patents
Manufacturing method for core-shell structure CdSe/CdS nanocrystalline for photovoltaic device Download PDFInfo
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Abstract
The invention discloses a manufacturing method for core-shell structure CdSe/CdS nanocrystalline for a photovoltaic device and aims at providing an improved water-phase synthesis technology. The key point of the technical scheme is that on the basis of an original technology, the surface photovoltaic property of the material is improved by a proper treatment method. Compared with a traditional manufacturing method, the manufacturing method disclosed by the invention has the characteristics that the wavelength range of a surface photovoltaic response of the obtained surface is widened by about 250 nanometers and is respectively positioned within a wavelength range of visible light; and the surface photovoltaic response strength of the sample is improved by about 6-25 times. The core-shell structure CdSe/CdS nanocrystalline disclosed by the invention has main purposes of improving the surface photovoltaic properties of key materials in photovoltaic devices and increasing the photovoltaic conversion efficiency of the photovoltaic device.
Description
Technical field
The present invention relates to inorganic non-metallic photovoltaic material preparing technical field, particularly for photovoltaic device there is the nanocrystalline a kind of preparation method of nucleocapsid structure cadmium selenide/CdS semiconduct.
Background technology
Semiconductor nanocrystal (also known as quantum dot) applies quantum limit on three dimension scale, electron system is made to have the kinestate of class atomic level, the i.e. kinestate complete quantization of microcosmic particle in quantum dot, and get discrete fixed electron energy state, this special structure makes the interaction of light and material more effective.Nucleocapsid structure cadmium selenide/CdS nanocrystal belongs to II/VI race semiconductor material, as shown in Figure 1, the nucleocapsid structure of this uniqueness imply that this material has more excellent functional performance and application prospect widely in fields such as photoelectron, microelectronics and solar photovoltaic devices to its nucleocapsid structure.
Summary of the invention
The object of the invention is the preparation method in order to provide a kind of nucleocapsid structure CdSe/CdS semiconductor nano, the present invention is achieved by the following technical solutions:
For the preparation method that photovoltaic device nucleocapsid structure CdSe/CdS is nanocrystalline, its concrete preparation process is as follows:
(1) the preparation of sodium hydrogen selenide
Add deionized water in a reservoir, then add selenium powder and sodium borohydride that mol ratio is 1:2.5, in nitrogen environment, under magnetic agitation, room temperature reaction is to the clarification of black selenium powder disappearance solution, and obtained sodium hydrogen selenide (NaHSe) aqueous solution, seals for subsequent use;
(2) the preparation of cadmium precursor solution
Cumulative volume when reacting with cadmium and selenium and cadmium concentration are for standard, be that Cadmium chloride fine powder and the sulfhydryl compound of 1:2 joins in deionized water by mol ratio, then the ratio in 2mol/L in above-mentioned mixed solution adds sodium hydroxide solution, makes the pH value of its mixed solution be adjusted to certain value;
Described step (2) in: cadmium source is Cadmium chloride fine powder, and different sulfhydryl compound and cadmium concentration proportioning are respectively: cadmium concentration got by Cadmium chloride fine powder/Thiovanic acid mixed solution is 0.1mol/L; Cadmium concentration got by Cadmium chloride fine powder/thiohydracrylic acid mixed solution is 0.05mol/L; Cadmium concentration got by Cadmium chloride fine powder/halfcystine mixed solution is 0.09mol/L;
Described step (2) middle pH value is:
Scheme 1; Cadmium chloride fine powder/Thiovanic acid mixed solution pH value is first adjusted to 6.0;
Scheme 2: Cadmium chloride fine powder/Thiovanic acid mixed solution pH value is adjusted to 9.5 or 11; Cadmium chloride fine powder/thiohydracrylic acid pH value is adjusted to 10.5; Cadmium chloride fine powder/halfcystine pH value is adjusted to 12;
(3) synthesize the coated nucleocapsid structure CdSe/CdS semiconductor nano of sulfydryl
Get step (2) in solution to four container in, under magnetic agitation, logical nitrogen removes the oxygen in reaction solution, under nitrogen protection, with cadmium source: selenium source mol ratio be 1:0.5 implantation step (1) in sodium hydrogen selenide solution in, react 0.5 hour under room temperature, be rapidly heated to 100 DEG C afterwards, reflux time is 2 ~ 4 hours, obtain the CdSe nanocrystalline colloidal sol that sulfydryl is coated, nanocrystalline with acetone precipitation CdSe, deionized water is separated with ethanol mixing, washing, afterwards by isolated throw out under 65 DEG C of conditions dry 7 hours, obtain the zinc blende-type CdSe/CdS core-shell nano crystalline flour end that photovoltaic response scope is 300 ~ 550nm or 600nm,
Above-mentioned steps (3) in, step (2) in scheme 1 and the difference of scheme 2 in treatment process be: scheme 1 added selenium source room temperature reaction after 0.5 hour, add the pH value to 11 regulating mixed solution in the sodium hydroxide solution of 2mol/L again, be warming up to 100 DEG C afterwards.
Above-mentioned steps (3) in: the reflux time in different sulfhydryl compound situation is, Cadmium chloride fine powder/Thiovanic acid backflow 2 or 3 hours; Cadmium chloride fine powder/thiohydracrylic acid refluxes 4 hours; Cadmium chloride fine powder/halfcystine refluxes 3 hours;
(4) wurtzite-type CdSe/CdS nucleocapsid structure semiconductor nano is prepared in thermal treatment
With the temperature rise rate of 5 DEG C/min, by step (3) in CdSe manocrystalline powders be put in and be rapidly heated in stove, rise to 450 ~ 500 DEG C from 20 DEG C, be incubated 1 ~ 3 hour, the cooling of sampling room temperature, obtains photovoltaic response scope brilliant from the wurtzite CdSe/CdS core-shell nano of 300 ~ 800nm.
Above-mentioned steps (4) in, soaking time raises corresponding minimizing with temperature, as 450 DEG C insulation 3 hours, 475 DEG C insulation 2 hours, 500 DEG C insulation 1 hour.
The present invention is a kind of water phase synthesis method of improvement.The detection of photovoltaic effect utilizes material by after illumination, and the separation of photoproduction free charge current carrier in surface and interface space charge region and diffusion, cause the change of surface potential barrier, i.e. surface photovoltaic spectroscopy.This technology studies the very effective detection means of one of semiconductor material photo-generated carrier transport behavior and electronic structure at present.
Owing to adopting technique scheme, a kind of preparation method nanocrystalline for photovoltaic device nucleocapsid structure CdSe/CdS provided by the invention, having such beneficial effect is: compared with traditional method, and the nucleocapsid structure CdSe/CdS nanocrystalline material adopting the present invention to prepare has:
(1) surface photovoltage responding range increase about 250 nanometer, and be all in visible-range;
(2) photovoltaic response maximum of intensity is 9.6mV, increase about 6 ~ 25 times compared with the photovoltaic response intensity obtaining sample with former traditional method.
Accompanying drawing explanation
Fig. 1. nucleocapsid structure CdSe/CdS nanocrystal submodel schematic diagram;
Fig. 2. in (A), curve is in example 1, when pH value is 11, backflow 3h obtains zinc blende-type nucleocapsid structure CdSe/CdS manocrystalline powders X-ray diffraction (XRD) spectrogram, wherein: the PDF card typical curve of-line representative cube CdS,--the PDF card typical curve of line representative cube CdSe; (B) in, curve is in example 1, when pH value is 11, it is last that backflow 3h obtains zinc blende-type nucleocapsid structure CdSe/CdS nanometer crystal powder, wurtzite-type nucleocapsid structure CdSe/CdS manocrystalline powders XRD spectra is obtained after sample 500 DEG C of thermal treatment insulation 1h, wherein: Δ Δ Δ line represents the PDF card typical curve of six side CdS, the PDF card typical curve of line representative cube CdO (being considered as dephasign); line represents the PDF card typical curve of six side CdSe;
Fig. 3. curve a in (A)
1and a
2when being respectively that in example 1, pH value is 11 and 9.5, the surface photovoltaic spectroscopy (SPS) that the zinc blende-type nucleocapsid structure CdSe/CdS that backflow 3h obtains is nanocrystalline; (B) curve b in (C) (D)
1, c
1and d
1when being respectively that in example 1, pH value is 11, the zinc blende-type CdSe/CdS nuclear shell structured nano-crystalline substance that obtains of backflow 3h respectively 450 DEG C, 475 DEG C, 500 DEG C thermal treatments, the SPS of the wurtzite-type CdSe/CdS nuclear shell structured nano-crystalline substance that each self-heat conserving 3h, 2h, 1h obtain; Curve b
2, c
2and d
2when being respectively that in example 1, pH value is 9.5, the zinc blende-type nucleocapsid structure CdSe/CdS that backflow 3h obtains is nanocrystalline respectively 450 DEG C, 475 DEG C, 500 DEG C thermal treatments, the SPS of the wurtzite-type CdSe/CdS nuclear shell structured nano-crystalline substance that each self-heat conserving 3h, 2h, 1h obtain;
Fig. 4. curve a is the nanocrystalline SPS of zinc blende-type nucleocapsid structure CdSe/CdS of preparation in example 2; Curve b, c and d are respectively 450 DEG C, 475 DEG C, 500 DEG C thermal treatments in example 2, the SPS that wurtzite-type nucleocapsid structure CdSe/CdS prepared by each self-heat conserving 3h, 2h, 1h is nanocrystalline;
Fig. 5. curve a is the nanocrystalline SPS of zinc blende-type nucleocapsid structure CdSe/CdS of preparation in example 3; Curve b, c and d are respectively 450 DEG C, 475 DEG C, 500 DEG C thermal treatments in example 3, the SPS that wurtzite-type nucleocapsid structure CdSe/CdS prepared by each self-heat conserving 3h, 2h, 1h is nanocrystalline;
Fig. 6. curve a is the nanocrystalline SPS of zinc blende-type nucleocapsid structure CdSe/CdS of preparation in example 4; Curve b, c and d are respectively 450 DEG C, 475 DEG C, 500 DEG C thermal treatments in example 4, the SPS that wurtzite-type nucleocapsid structure CdSe/CdS prepared by each self-heat conserving 3h, 2h, 1h is nanocrystalline.
Embodiment:
Below in conjunction with accompanying drawing and embodiment, the present invention is described in further detail:
Wherein the adjustment of example 2pH value adopts the scheme 1 described in summary of the invention step; Other example pH value regulates and is scheme 2.
Embodiment 1
(1) getting 20mL deionized water adds in the triangular flask of 50mL, and under magnetic agitation, add 1.253g sodium borohydride and 0.869g selenium powder, react about 15min under nitrogen protection, obtain water white NaHSe solution, adularescent crystallization sucking-off, seals for subsequent use;
(2) Cadmium chloride fine powder of 5.024g and the Thiovanic acid of 4.054g are joined in the beaker of 155mL deionized water, above-mentioned mixed solution pH value is regulated to be 9.5 (add 43.5mL by the NaOH solution of 2mol/L, the NaOH of 2mol/L) or 11 (add 46.5mL, the NaOH of 2mol/L), cadmium-sulfydryl mixed solution is moved in four-hole boiling flask, logical nitrogen 25min is except oxygen in mixed solution, add rapidly the NaHSe solution in (1) step, under nitrogen protection, room temperature reaction 0.5h, be warming up to 100 DEG C, backflow 3h, obtains CdSe colloidal sol;
(3) by the CdSe colloidal sol acetone precipitation in (2), get precipitated liquid dehydrated alcohol and deionized water wash centrifugation 3 times, be put in 65 DEG C of dry 7h in baking oven afterwards, obtaining photovoltaic response scope is that the zinc blende-type nucleocapsid structure CdSe/CdS of 300 ~ 550nm is nanocrystalline;
(4) a certain amount of zinc blende-type CdSe/CdS manocrystalline powders obtained in (3) is got, be put in and be energy-savingly rapidly heated in stove, 20 DEG C start with the heat-up rate of 5 DEG C/min, rise to 450 DEG C, 475 DEG C, 500 DEG C respectively, each self-heat conserving 3h, 2h, 1h, the cooling of sampling room temperature, obtaining photovoltaic response scope is that the wurtzite-type nucleocapsid structure CdSe/CdS of 300 ~ 800nm is nanocrystalline.
Embodiment 2
(1) getting 20mL deionized water adds in the triangular flask of 50mL, under magnetic agitation, adds 1.253g sodium borohydride and 0.869g selenium powder, reacts about 15min under nitrogen protection, obtain water white NaHSe solution, adularescent crystallization, seal for subsequent use;
(2) Cadmium chloride fine powder of 5.024g and the Thiovanic acid of 4.054g are joined in the beaker of 155mL deionized water, (40mL is added by the NaOH solution adjust ph to 6.0 of 2mol/L, the NaOH of 2mol/L), logical nitrogen 25min is except oxygen in mixed solution, add rapidly the NaHSe solution in (1) step afterwards, room temperature reaction 0.5h under nitrogen protection, continue afterwards to regulate mixed solution pH value (to add 5.5mL to 11, the NaOH of 2mol/L), mixed solution is moved in four-hole boiling flask, be warming up to 100 DEG C under nitrogen protection, backflow 2h, obtains CdSe colloidal sol;
(3) by the CdSe colloidal sol acetone precipitation in (2), taking precipitate dehydrated alcohol and deionized water wash centrifugation 3 times, to be put in baking oven dry 7h at 65 DEG C afterwards, obtaining photovoltaic response scope is that the zinc blende-type nucleocapsid structure CdSe/CdS of 300 ~ 550nm is nanocrystalline;
(4) a certain amount of zink sulphide CdSe/CdS manocrystalline powders obtained in (3) is got, be put in and be energy-savingly rapidly heated in stove, 20 DEG C start with the heat-up rate of 5 DEG C/min, rise to 450 DEG C, 475 DEG C, 500 DEG C respectively, each self-heat conserving 3h, 2h, 1h, the cooling of sampling room temperature, obtaining photovoltaic response scope is that the wurtzite-type nucleocapsid structure CdSe/CdS of 300 ~ 800nm is nanocrystalline.
Embodiment 3
(1) getting 7mL deionized water adds in the triangular flask of 50mL, under magnetic agitation, adds 0.256g sodium borohydride and 0.214g selenium powder, reacts about 20min under nitrogen protection, obtain water white NaHSe solution, seal for subsequent use;
(2) Cadmium chloride fine powder of 1.233g and the Cys of 1.309g are joined in the beaker of 35mL deionized water, by the NaOH solution adjust ph to 12 of 2mol/L, (add 20mL, the NaOH of 2mol/L), logical nitrogen 20min, except oxygen in mixed solution, adds rapidly the NaHSe solution in (1) step afterwards, room temperature reaction 0.5h under nitrogen protection, be warming up to 100 DEG C, backflow 3h, obtains CdSe colloidal sol;
(3) by the CdSe colloidal sol acetone precipitation in (2), taking precipitate dehydrated alcohol and deionized water wash centrifugation 3 times, to be put in baking oven dry 7h at 65 DEG C afterwards, obtaining photovoltaic response scope is that the zinc blende-type nucleocapsid structure CdSe/CdS of 300 ~ 600nm is nanocrystalline;
(4) a certain amount of zink sulphide CdSe/CdS manocrystalline powders obtained in (3) is got, be put in and be energy-savingly rapidly heated in stove, 20 DEG C start with the heat-up rate of 5 DEG C/min, rise to 450 DEG C, 475 DEG C, 500 DEG C respectively, each self-heat conserving 3h, 2h, 1h, the cooling of sampling room temperature, obtaining photovoltaic response scope is that the wurtzite-type nucleocapsid structure CdSe/CdS of 300 ~ 800nm is nanocrystalline.
Embodiment 4
(1) getting 10mL deionized water adds in the triangular flask of 50mL, under magnetic agitation, adds 0.142g sodium borohydride and 0.119g selenium powder, reacts about 23min under nitrogen protection, obtain water white NaHSe solution, seal for subsequent use;
(2) Cadmium chloride fine powder of 0.685g and the thiohydracrylic acid of 0.637g are joined in the beaker of 45mL deionized water, (6.2mL is added by the NaOH solution adjust ph to 10.5 of 2mol/L, the NaOH of 2mol/L), logical nitrogen 20min is except oxygen in mixed solution, add rapidly the NaHSe solution in (1) step, room temperature reaction 0.5h under nitrogen protection, is warming up to 100 DEG C, backflow 4h, obtains CdSe colloidal sol;
(3) by the CdSe colloidal sol acetone precipitation in (2), taking precipitate dehydrated alcohol and deionized water wash centrifugation 3 times, to be put in baking oven dry 7h at 65 DEG C afterwards, obtaining photovoltaic response scope is that the zinc blende-type nucleocapsid structure CdSe/CdS of 300 ~ 550nm is nanocrystalline;
(4) a certain amount of zink sulphide CdSe/CdS manocrystalline powders obtained in (3) is got, be put in and be energy-savingly rapidly heated in stove, 20 DEG C start with the heat-up rate of 5 DEG C/min, rise to 450 DEG C, 475 DEG C, 500 DEG C respectively, each self-heat conserving 3h, 2h, 1h, the cooling of sampling room temperature, obtaining photovoltaic response scope is that the wurtzite-type nucleocapsid structure CdSe/CdS of 300 ~ 800nm is nanocrystalline.
Claims (4)
1. for the preparation method that photovoltaic device nucleocapsid structure CdSe/CdS is nanocrystalline, it is characterized in that: its concrete preparation process is as follows:
(1) the preparation of sodium hydrogen selenide
Add deionized water in a reservoir, then add selenium powder and sodium borohydride that mol ratio is 1:2.5, in nitrogen environment, under magnetic agitation, room temperature reaction is to the clarification of black selenium powder disappearance solution, and the obtained sodium hydrogen selenide aqueous solution, seals for subsequent use;
(2) the preparation of cadmium precursor solution
Cumulative volume when reacting with cadmium and selenium and cadmium concentration are for standard, be that Cadmium chloride fine powder and the sulfhydryl compound of 1:2 joins in deionized water by mol ratio, then the ratio in 2mol/L in above-mentioned mixed solution adds sodium hydroxide solution, makes the pH value of its mixed solution be adjusted to certain value;
Its pH value is:
Scheme 1; Cadmium chloride fine powder/Thiovanic acid mixed solution pH value is first adjusted to 6.0;
Scheme 2: Cadmium chloride fine powder/Thiovanic acid mixed solution pH value is adjusted to 9.5 or 11; Cadmium chloride fine powder/thiohydracrylic acid pH value is adjusted to 10.5; Cadmium chloride fine powder/halfcystine pH value is adjusted to 12;
(3) synthesize the coated nucleocapsid structure CdSe/CdS semiconductor nano of sulfydryl
Get step (2) in solution to four container in, under magnetic agitation, logical nitrogen removes the oxygen in reaction solution, under nitrogen protection, with cadmium source: selenium source mol ratio be 1:0.5 implantation step (1) in sodium hydrogen selenide solution in, react 0.5 hour under room temperature, be rapidly heated to 100 DEG C afterwards, the reflux time in different sulfhydryl compound situation is, Cadmium chloride fine powder/Thiovanic acid backflow 2 or 3 hours; Cadmium chloride fine powder/thiohydracrylic acid refluxes 4 hours; Cadmium chloride fine powder/halfcystine refluxes 3 hours; Obtain the CdSe nanocrystalline colloidal sol that sulfydryl is coated, nanocrystalline with acetone precipitation CdSe, deionized water is separated with ethanol mixing, washing, afterwards by isolated throw out under 65 DEG C of conditions dry 7 hours, obtain the zinc blende-type CdSe/CdS core-shell nano crystalline flour end that photovoltaic response scope is 300 ~ 550nm or 600nm;
(4) wurtzite-type CdSe/CdS nucleocapsid structure semiconductor nano is prepared in thermal treatment
With the temperature rise rate of 5 DEG C/min, by step (3) in CdSe manocrystalline powders be put in and be rapidly heated in stove, rise to 450 ~ 500 DEG C from 20 DEG C, be incubated 1 ~ 3 hour, the cooling of sampling room temperature, obtains photovoltaic response scope brilliant from the wurtzite CdSe/CdS core-shell nano of 300 ~ 800nm.
2. a kind of preparation method nanocrystalline for photovoltaic device nucleocapsid structure CdSe/CdS according to claim 1, it is characterized in that: step (2) in: described cadmium source is Cadmium chloride fine powder, and different sulfhydryl compound and cadmium concentration proportioning are respectively: cadmium concentration got by Cadmium chloride fine powder/Thiovanic acid mixed solution is 0.1mol/L; Cadmium concentration got by Cadmium chloride fine powder/thiohydracrylic acid mixed solution is 0.05mol/L; Cadmium concentration got by Cadmium chloride fine powder/halfcystine mixed solution is 0.09mol/L.
3. a kind of preparation method nanocrystalline for photovoltaic device nucleocapsid structure CdSe/CdS according to claim 1, it is characterized in that: step (3) in, step (2) in scheme 1 and scheme 2 in the difference for the treatment of process be: scheme 1 added selenium source room temperature reaction after 0.5 hour, add the pH value to 11 regulating mixed solution in the sodium hydroxide solution of 2mol/L again, be warming up to 100 DEG C afterwards.
4. a kind of preparation method nanocrystalline for photovoltaic device nucleocapsid structure CdSe/CdS according to claim 1, it is characterized in that: step (4) in, soaking time raises corresponding minimizing with temperature, and holding temperature and soaking time are that 450 DEG C of insulations 3 hours or 475 DEG C of insulations are incubated 1 hour in 2 hours or 500 DEG C.
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| CN112391648B (en) * | 2020-10-22 | 2022-03-01 | 中国科学技术大学 | Photo-anode material with low initial potential and preparation method thereof |
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| Synthesis and Characterization of Thio Capped CdSe and CdSe/CdS Core Shell Nanocrystals in Aqueous Solution;AN Li Ming;《Nanotechnology and precision engineering》;20040930;第2卷(第3期);全文 * |
| 水溶性CdSe/CdS纳米晶合成条件的优化研究;钟萍等;《化学研究与应用》;20060330;第18卷(第3期);全文 * |
| 水相中CdSe与核/壳CdSe/CdS量子点的制备与发光特性研究;唐爱伟等;《无机材料学报》;20060331;第21卷(第2期);全文 * |
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