CN103904167A - Method for preparing CdSxSey photoelectric material - Google Patents

Method for preparing CdSxSey photoelectric material Download PDF

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CN103904167A
CN103904167A CN201410163697.4A CN201410163697A CN103904167A CN 103904167 A CN103904167 A CN 103904167A CN 201410163697 A CN201410163697 A CN 201410163697A CN 103904167 A CN103904167 A CN 103904167A
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solution
cds
cdsxsey
colloid
photoelectric material
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CN103904167B (en
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钟福新
王伟
黎燕
莫德清
王丹宇
王苏宁
朱义年
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Nanjing Xiaoyi Information Technology Co ltd
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Guilin University of Technology
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104Forming layers
    • H01L21/02365Forming inorganic semiconducting materials on a substrate
    • H01L21/02367Substrates
    • H01L21/0237Materials
    • H01L21/02425Conductive materials, e.g. metallic silicides
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104Forming layers
    • H01L21/02365Forming inorganic semiconducting materials on a substrate
    • H01L21/02518Deposited layers
    • H01L21/02521Materials
    • H01L21/02551Group 12/16 materials
    • H01L21/0256Selenides
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104Forming layers
    • H01L21/02365Forming inorganic semiconducting materials on a substrate
    • H01L21/02612Formation types
    • H01L21/02617Deposition types
    • H01L21/02623Liquid deposition
    • H01L21/02628Liquid deposition using solutions
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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  • Condensed Matter Physics & Semiconductors (AREA)
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Abstract

The invention discloses a method for preparing a CdSxSey photoelectric material. The method comprises the steps that (1) 0.1079-0.1349 g of KBH4 is added to a 0.04-0.05 mol/L Na2SeO3 solution of 5 mL and a solution A is obtained through stirring the mixture under a water bath at the temperature of 30 DEG C to 40 DEG C; (2) 0.0394-0.0789 g of citric acid is added to a 0.04-0.05 mol/L Cd(NO3)2 solution of 5 mL so that a solution B can be prepared; (3) the solution A and the solution B are mixed, 0.0152-0.0229 g of CH4N2S is added to the mixture of the solution A and the solution B for dissolution so that a solution C can be obtained; (4) the solution C reacts for eight to ten hours in a thermostat at the temperature of 120 DEG C to 160 DEG C and a CdSxSey colloid is obtained, wherein x ranges from 0.43 to 0.48 and y ranges from 0.52 to 0.57; (5) the CdSxSey colloid serves as epoxy resin in an ice-water bath at 0 DEG C, heat treatment is conducted on conductive glass ITO for 20 minutes at the temperature of 90 DEG C, the conductive glass ITO serves as a hot medium, the ITO conductive face is coated with the CdSxSey through a cold-heat alternating coating method, and coating operation lasts for one minute; coating operation is repeated twice to five times. The method is low in cost, short in treatment time and free of pollution, the technology is convenient, and the obtained CdSxSey photoelectric material is good in photoelectric performance.

Description

A kind of CdS xse ythe preparation method of photoelectric material
Technical field
The present invention relates to a kind of CdS xse ythe preparation method of photoelectric material.
Background technology
Because charge carrier number in intrinsic semiconductor is few, photoconduction power is very low, if but mix therein micro-impurity, the photoconductivity of the extrinsic semiconductor forming can will strengthen greatly, so doping can change semi-conductive fundamental characteristics completely, can effectively control optical, electrical, the magnetic characteristic of semiconductor nanocrystal, directly cause the realization of the photoelectron devices such as high efficiency light-emitting device, rare magnetic spin electronic device, solar cell, for the extensive use of nanocrystal provides huge space.
CdSe is as II~VI compound semiconductor of direct band gap, have leakage current little, be difficult for deliquescence, good photoconductive property, be a kind of fabulous indoor temperature nucleus radiation detecting material.The people such as T.P.Brody are successfully developed into liquid crystal and the electroluminescent display of CdSe-TFT active matrix addressing, make CdSe aspect thin-film transistor, present wide application prospect.CdSe has cube and two kinds of structures of six sides, because of have with solar spectrum in the suitable bandwidth of visible light wave range (<1.7ev), therefore CdSe is the important source material of making heterojunction solar cell and photoelectrochemical solar cell.But but exist charge carrier number few as intrinsic semiconductor CdSe, the problem that photoconduction power is low, optical, electrical, the magnetic characteristic of mixing a certain amount of impurity and can effectively control CdSe nanocrystal, directly cause CdSe photoconductivity to strengthen.At present CdSe doping type mainly contains solvent-thermal method and prepares that Zn doping CdSe is nanocrystalline is conducive to improve its application aspect opto-electronic device, laser diode and other photochemistry and electrochemistry, electrochemical production Co doping CdSe film is conducive to the raising of photoelectric catalysis degrading performance, and the synthetic lead ion doping CdSe quantum dot of water method has good fluorescent characteristic.The research of CdSe doping vario-property becomes a focus, and that CdSe is entrained in the research of photoelectric conversion aspect of performance is actually rare.S also has a small amount of report at present to the doping of CdSe, as Pan Anlian etc. is combined with each other CdS and CdSe by the synthetic method of high temperature vapour phase, obtains CdS xse yternary alloy three-partalloy; Yu Chong etc. are by the wider CdS of chemical vapour deposition technique one-step synthesis nanobelt xse y.But these two kinds of method synthesis conditions are harsher, not easy to operate, the CdS simultaneously obtaining xse ymixed crystal degree is larger, and it is wayward that S mixes concentration.And hydro thermal method is prepared CdS xse yphotoelectric material there is not yet report.This technique simply, does not produce pollution, synthetic CdS xse ypresent colloidal and be convenient to prepare photoelectric device.Gained CdS xse yopen circuit photovoltage also larger, be a kind of photoelectric material preferably, be expected to as solar photocell material.
Summary of the invention
The object of this invention is to provide a kind of with the hydro-thermal legal system CdS that got everything ready xse y,the method of photoelectric material, wherein x=0.43~0.48, y=0.52~0.57.
Concrete steps are:
(1) be 0.04 ~ 0.05mol/L Na to 5mL concentration 2seO 3in solution, add 0.1079 ~ 0.1349g KBH 4, 30 ~ 40 ℃ of lower magnetic forces of water-bath stir and within 5 ~ 6 minutes, are mixed with A solution, control Na 2seO 3with KBH 4mol ratio=1:10.
(2) be 0.04 ~ 0.05mol/L Cd (NO to 5mL concentration 3) 2in solution, add 0.0394 ~ 0.0789g citric acid to be mixed with B solution, control Cd (NO 3) 2with citric acid mol ratio=1:1.
(3) under magnetic agitation, A solution mixes completely with B solution, and controlling Se:Cd mol ratio is 1:1, then adds 0.0152 ~ 0.0229g CH 4n 2s dissolves, and obtains C solution.
(4) C solution proceeds in hydrothermal reaction kettle, in 120 ~ 160 ℃ of insulating boxs, reacts 8 ~ 10 hours, and then cool to room temperature, obtains CdS xse ycolloid.
(5) by step (4) gained CdS xse ycolloid is placed in 0 ℃ of ice-water bath as epoxy resin, and electro-conductive glass ITO heat treatment in 90 ℃ of baking ovens adopts hot and cold alternately semar technique by CdS as hot material in 20 minutes xse yspread upon ITO conducting surface, smear 1 minute time.
(6) repeating step (5) 2 ~ 5 times, makes CdS xse yphotoelectric material, CdS under simulated solar irradiation xse yopen circuit photovoltage reach 0.2229 ~ 0.3678V.
The present invention is compared with other correlation technique, and outstanding feature is that hydro thermal method is prepared CdS xse ycolloid, and with hot and cold alternately semar technique by CdS xse ybe made into electrode.This preparation technology is easy, pollution-free, the CdS of preparation xse ysample has good photoelectric properties.
specific experiment method:
embodiment 1:
(1) be 0.04mol/L Na to 5mL concentration 2seO 3in solution, add 0.1079g KBH 4, 40 ℃ of lower magnetic forces of water-bath stir and within 5 minutes, are mixed with A solution.
(2) be 0.04mol/L Cd (NO to 5mL concentration 3) 2in solution, add 0.0394g citric acid to be mixed with B solution.
(3) under magnetic agitation, A solution and B solution are mixed completely, then add 0.019g CH 4n 2s dissolves, and obtains C solution.
(4) step (3) gained C solution is proceeded in hydrothermal reaction kettle, hydro-thermal reaction 8 hours in 120 ℃ of insulating boxs, then cool to room temperature, obtains CdS xse ycolloid.
(5) by step (4) gained CdS xse ycolloid is placed in 0 ℃ of ice-water bath and is cooled to epoxy resin, and electro-conductive glass ITO heat treatment in 90 ℃ of baking ovens adopts hot and cold alternately semar technique by CdS as hot material in 20 minutes xse yspread upon 1.8cm × 5cm × 0.11cm ITO conducting surface, smear 1 minute time.
(6) repeating step (5) 5 times, makes CdS xse yphotoelectric material, CdS under simulated solar irradiation xse yopen circuit photovoltage reach 0.2229V, the CdS of acquisition xse yin x=0.43, y=0.57.
embodiment 2:
(1) be 0.05mol/LNa to 5mL concentration 2seO 3in solution, add 0.1349g KBH 4, 30 ℃ of lower magnetic forces of water-bath stir and within 6 minutes, are mixed with A solution.
(2) be 0.05mol/L Cd (NO to 5mL concentration 3) 2in solution, add 0.0525g citric acid to be mixed with B solution.
(3) under magnetic agitation, A solution and B solution are mixed completely, then add 0.0152g CH 4n 2s dissolves, and obtains C solution.
(4) step (3) gained C solution is proceeded in hydrothermal reaction kettle, hydro-thermal reaction 8 hours in 120 ℃ of insulating boxs, then cool to room temperature, obtains CdS xse ycolloid.
(5) by step (4) gained CdS xse ycolloid is placed in 0 ℃ of ice-water bath and is cooled to epoxy resin, and ITO heat treatment in 90 ℃ of baking ovens adopts hot and cold alternately semar technique by CdS as hot material in 20 minutes xse yspread upon 1.8cm × 5cm × 0.11cm ITO conducting surface, smear 1 minute time.
(6) repeating step (5) 3 times, makes CdS xse yphotoelectric material, CdS under simulated solar irradiation xse yopen circuit photovoltage reach 0.3302V.Obtain CdS xse yin x=0.45, y=0.55.
embodiment 3:
(1) Na that is 0.04mol/L to 5mL concentration 2seO 3solution adds 0.1079g KBH 4, 40 ℃ of lower magnetic forces of water-bath stir and within 5 minutes, are mixed with A solution.
(2) Cd (NO that is 0.04mol/L to 5mL concentration 3) 2in solution, add 0.0394g citric acid to be mixed with B solution.
(3) under magnetic agitation, A solution and B solution are mixed completely, then add 0.019g CH 4n 2s dissolves, and obtains C solution.
(4) step (3) gained C solution is proceeded in hydrothermal reaction kettle, hydro-thermal reaction 10 hours in 120 ℃ of insulating boxs, then cool to room temperature, obtains CdS xse ycolloid.
(5) by step (4) gained CdS xse ycolloid is placed in 0 ℃ of ice-water bath cooling condensation glue, and ITO heat treatment in 90 ℃ of baking ovens adopts hot and cold alternately semar technique by CdS as hot material in 20 minutes xse yspread upon 1.8cm × 5cm × 0.11cm ITO conducting surface, smear 1 minute time.
(6) repeating step (5) 5 times, makes CdS xse yphotoelectric material, CdS under simulated solar irradiation xse yopen circuit photovoltage reach 0.3177V.Obtain CdS xse yin x=0.47, y=0.53.
embodiment 4:
(1) be 0.05mol/LNa to 5mL concentration 2seO 3in solution, add 0.1349g KBH 4, 30 ℃ of lower magnetic forces of water-bath stir and within 5 minutes, are mixed with A solution.
(2) be 0.05mol/L Cd (NO to 5mL concentration 3) 2in solution, add 0.0525g citric acid to be mixed with B solution.
(3) under magnetic agitation, A solution and B solution are mixed completely, then add 0.019g CH 4n 2s dissolves, and obtains C solution.
(4) step (3) gained C solution is proceeded in hydrothermal reaction kettle, hydro-thermal 10 hours in 160 ℃ of insulating boxs, then cool to room temperature, obtains CdS xse ycolloid.
(5) by step (4) gained CdS xse ycolloid is placed in 0 ℃ of ice-water bath and is cooled to epoxy resin, and ITO heat treatment in 90 ℃ of baking ovens adopts hot and cold alternately semar technique by CdS as hot material in 20 minutes xse yspread upon 1.8cm × 5cm × 0.11cm ITO conducting surface, smear 1 minute time.
(6) repeating step (5) 2 times, makes CdS xse yphotoelectric material, CdS under simulated solar irradiation xse yopen circuit photovoltage reach 0.3678V.Obtain CdS xse yin x=0.48, y=0.52.

Claims (1)

1. a CdS xse ythe preparation method of photoelectric material, wherein x=0.43~0.48, y=0.52~0.57, is characterized in that concrete steps are:
(1) be 0.04 ~ 0.05mol/L Na to 5mL concentration 2seO 3in solution, add 0.1079 ~ 0.1349g KBH 4, 30 ~ 40 ℃ of lower magnetic forces of water-bath stir and within 5 ~ 6 minutes, are mixed with A solution, control Na 2seO 3with KBH 4mol ratio=1:10;
(2) be 0.04 ~ 0.05mol/L Cd (NO to 5mL concentration 3) 2in solution, add 0.0394 ~ 0.0789g citric acid to be mixed with B solution, control Cd (NO 3) 2with citric acid mol ratio=1:1;
(3) under magnetic agitation, A solution mixes completely with B solution, and controlling Se:Cd mol ratio is 1:1, then adds 0.0152 ~ 0.0229g CH 4n 2s dissolves, and obtains C solution;
(4) step (3) gained C solution is proceeded in hydrothermal reaction kettle, in 120 ~ 160 ℃ of insulating boxs, react 8 ~ 10 hours, then cool to room temperature, obtains CdS xse ycolloid;
(5) by step (4) gained CdS xse ycolloid is placed in 0 ℃ of ice-water bath as epoxy resin, and electro-conductive glass ITO heat treatment in 90 ℃ of baking ovens adopts hot and cold alternately semar technique by CdS as hot material in 20 minutes xse yspread upon ITO conducting surface, smear 1 minute time;
(6) repeating step (5) 2 ~ 5 times, makes CdS xse yphotoelectric material, wherein x=0.43~0.48, y=0.52~0.57.
CN201410163697.4A 2014-04-23 2014-04-23 A kind of CdS xse ythe preparation method of photoelectric material Active CN103904167B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104952961A (en) * 2015-06-18 2015-09-30 常熟理工学院 n-CdSxSe1-x film/graphene schottky junction solar cell
CN106409961A (en) * 2016-11-23 2017-02-15 常熟理工学院 N-Si/CdSSe laminated solar cell and preparation method thereof

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CN102522454A (en) * 2011-12-15 2012-06-27 广东工业大学 Preparation method of CdSe nanocrystal semiconductor film
US20130174778A1 (en) * 2012-01-06 2013-07-11 Iowa State University Research Foundation, Inc. Controlled Fabrication of Semiconductor-Metal Hybrid Nano-Heterostructures via Site-Selective Metal Photodeposition

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CN102522454A (en) * 2011-12-15 2012-06-27 广东工业大学 Preparation method of CdSe nanocrystal semiconductor film
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104952961A (en) * 2015-06-18 2015-09-30 常熟理工学院 n-CdSxSe1-x film/graphene schottky junction solar cell
CN106409961A (en) * 2016-11-23 2017-02-15 常熟理工学院 N-Si/CdSSe laminated solar cell and preparation method thereof
CN106409961B (en) * 2016-11-23 2018-06-29 常熟理工学院 n-Si/CdSSe laminated solar cell and preparation method thereof

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