CN101979723B - Method for preparing p-type CdS nanowires - Google Patents

Method for preparing p-type CdS nanowires Download PDF

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CN101979723B
CN101979723B CN2010105554956A CN201010555495A CN101979723B CN 101979723 B CN101979723 B CN 101979723B CN 2010105554956 A CN2010105554956 A CN 2010105554956A CN 201010555495 A CN201010555495 A CN 201010555495A CN 101979723 B CN101979723 B CN 101979723B
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nano wire
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CN101979723A (en
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王春瑞
蔡俊晟
徐靖
王洪云
叶茂林
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Donghua University
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Abstract

The invention relates to a method for preparing p-type CdS nanowires. The method comprises the following steps of: (1) blending CdS powder and Sn powder in a mass ratio of 2-4:1, adding the mixture on an aluminum oxide boat of a tube furnace and placing a p-type aluminum oxide boat in the downwind direction of the raw materials; (2) continuously vacuumizing to control the pressure in the furnace to be between 200 and 300Torr and introducing argon gas of which the flow rate is 50 to 100sccm at the same time; and (3) controlling the central temperature of a reaction tube to be between 800 and 900 DEG C, and after keeping the temperature for 2 to 4 hours, naturally cooling the product to room temperature to obtain the p-type CdS nanowires. The preparation process of the invention is simple and feasible and can be finished in one step; the repeatability is high; the difficulty of preparing the p-type CdS nanowires is overcome; the stability is high; and the product is expected to greatly promote the development of CdS nanowire-based photoelectric devices, particularly solve the technical problem of wide band-gap II-VI semiconductor material p-type doping.

Description

A kind of preparation method of p type CdS nano wire
Technical field
The invention belongs to the preparation field of CdS nano wire, particularly a kind of preparation method of p type CdS nano wire.
Background technology
In recent years, one-dimensional nano structure material because of its with block materials different unique optics, electrical properties, caused people's extensive interest.They not only provide the ideal system of the low dimension of a research object physical properties, also are the important structure unit of constructing nanoscale electric, photonic device.
CdS is the wide bandgap semiconductor materials of a kind of II-VI family; Its energy gap is 2.4eV under the room temperature; At present, the research aspect of CdS one dimension Nano structure has obtained certain progress, on photodiode, solar cell or other photoelectric device, the potential application prospect is arranged.But because the semi-conductive self compensation effect of II-VI family, the p type doping problem of CdS nano wire is focus, the difficult point that people study always.Be easy to generate various donor-type defectives in intrinsic CdS nano wire inside, auto-compensation take place make p type CdS nano wire be difficult to preparation.This has restricted the application of CdS nano wire aspect photoelectric device to a great extent.Though V group element such as N, P doping CdS nano wire presents p type electroconductibility, and V group element doping CdS stability is poor.Therefore, the preparation method who explores p type CdS nano wire is that to be badly in need of very much also be very challenging.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of p type CdS nano wire, and preparation is simple in this invention, adopts single stage method to accomplish, and good reproducibility has overcome difficulty and good stability that p type CdS nano wire prepares; Products therefrom is expected to advance greatly the development based on CdS nano wire photoelectric device, particularly is expected to solve the adulterated technical barrier of broad-band gap II-VI semiconductor material p type.
The preparation method of a kind of p type CdS nano wire of the present invention comprises:
(1) with CdS powder and Sn powder by mass ratio 2~4: 1 mixes and places on the aluminium sesquioxide boat of tube furnace, is substrate with p type silicon substrate, puts into the aluminium sesquioxide boat of starting material leeward;
(2) continuing to vacuumize the control furnace pressure is 200~300Torr (1Torr ≈ 133Pa), feeds the argon gas that flow is 50~100sccm simultaneously;
(3) control reaction tubes central authorities temperature is 800~900 ℃, behind insulation 2~4h, naturally cools to room temperature, promptly gets.
Said p type silicon substrate model is 100, the surface be coated with thickness be 50
Figure BDA0000033852670000011
golden film.
Beneficial effect
(1) preparation is simple in the present invention, adopts single stage method to accomplish, and good reproducibility has overcome difficulty and good stability that p type CdS nano wire prepares;
(2) products therefrom of the present invention is expected to advance greatly the development based on CdS nano wire photoelectric device, particularly is expected to solve the adulterated technical barrier of broad-band gap II-VI semiconductor material p type.
Description of drawings
Fig. 1 is the experimental installation synoptic diagram;
Fig. 2 is the alternating temperature photoluminescence spectrum of the CdS nano wire of preparation;
Fig. 3 is the X-ray diffractogram of the CdS nano wire of preparation; Wherein the diffraction peak of Si derives from substrate.
Fig. 4 is the electron scanning micrograph of the CdS nano wire of preparation;
Fig. 5 is the structural representation of p type CdS nanometer wire field effect tube;
Fig. 6 is the I with the FET of the CdS nano wire making of preparation Ds-V GsRational curve.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition those skilled in the art can do various changes or modification to the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
CdS and Sn powder mixed with 2: 1 mass ratio be placed on the reaction tubes mid-way.With p type (100) silicon substrate is substrate, places it in the about 30cm of the middle leeward of reaction tubes place aluminium sesquioxide boat reaction tubes one termination airing system; The other end connects mechanical pump, keep-ups pressure to be 300Torr (1Torr ≈ 133Pa), and continuing simultaneously to feed flow is the argon gas of 50~100sccm; Control reaction tubes central authorities temperature is 900 ℃ in the experiment, behind the insulation 2h, closes heating power supply; Naturally cool to room temperature, obtain yellow lint shape material.The sign of product utilization X-ray powder diffraction, sem (SEM) and photoluminescence spectrum (PL), electronic transport photoelectric properties test analysis, the product of preparation is the CdS nano wire, presents p type electroconductibility, promptly prepares p type CdS nano wire.Figure is X-ray powder diffraction, sem (SEM), photoluminescence spectrum (PL) and electronic transport Measurement results below.
Fig. 2 is sem (SEM) photo of the p type CdS nano wire of preparation.As can be seen from the figure product is wire, and diameter is a hundreds of nanometer to a micron, and length is several microns to tens microns.
Fig. 3 is the X-ray diffraction pattern (XRD) of the p type CdS nano wire corresponding with Fig. 2.All diffraction peaks among the figure can index be that (JCPDS 75-1545), has proved degree of purity of production to six side's phase CdS.
Fig. 4 is the alternating temperature photoluminescence spectrum (PL) of the p type CdS nano wire of preparation.Can observe in Fig. 4 illustration along with receiving main beam to tie up the evolutionary process at exciton peak in the variation of temperature photoluminescence spectrum; Along with constantly weakening at the alms giver-bound exciton peak and the free exciton peak of the rising product of temperature; And receive main beam to tie up exciton peak grow; Hint receives the main phenomenon that strengthens, and explains that the CdS nano wire presents p type electroconductibility.
Fig. 6 is the Ids-Vgs rational curve with the FET of the CdS nano wire making of preparation.The making of CdS nanometer wire field effect tube is based on shown in Figure 5, and the CdS nano wire that is about to preparation is distributed in the ethanolic soln, then it is dropped on the device substrate shown in Figure 5, after the seasoning on nano wire depositing electrode form device architecture shown in Figure 5.As can be seen from Figure 6, Ids increases with grid voltage Vgs and reduces, the characteristic that had of p channel field-effect pipe at this moment, and it is consistent with top optical performance test result prove that the CdS for preparing presents p N-type semiconductorN characteristic.
Through above-mentioned photoelectric properties test the result, prove that further this invention utilizes CdS and the prepared CdS nano wire of Sn coevaporation to present p type electroconductibility, promptly prepares p type CdS nano wire.The prepared product of the present invention was placed after 4 years, and measuring optical and electronic transport characteristic do not have considerable change, have proved the stability of product.Explaining that tin (Sn) is acceptor impurity in CdS, is effective doping agent of preparation p type CdS.
Other need to prove: (Sn) is stable acceptor impurity in CdS although the present invention proves tin, is effective doping agent of preparation p type CdS.But the bright related ways and means of we can not provide doping content or the content of Sn.
Embodiment 2
CdS and Sn powder mixed with 4: 1 mass ratio be placed on the reaction tubes mid-way.With p type (100) silicon substrate is substrate, puts into the aluminium sesquioxide boat at the about 30cm of starting material leeward place, reaction tubes one termination airing system; The other end connects mechanical pump, keep-ups pressure to be 200Torr (1Torr ≈ 133Pa), and continuing simultaneously to feed flow is the argon gas of 50~100sccm; Control reaction tubes central authorities temperature is 900 ℃ in the experiment, behind the insulation 3h, closes heating power supply; Naturally cool to room temperature, obtain yellow lint shape material.The sign of product utilization X-ray powder diffraction, sem (SEM) and photoluminescence spectrum (PL), electronic transport photoelectric properties test analysis, the product of preparation is the CdS nano wire, presents p type electroconductibility, promptly prepares p type CdS nano wire.There is not notable difference with structure, pattern and the photoelectric properties of CdS among the embodiment 1.
Embodiment 3
CdS and Sn powder mixed with 3: 1 mass ratio be placed on the reaction tubes mid-way.With p type (100) silicon substrate is substrate, puts into the aluminium sesquioxide boat at the about 30cm of starting material leeward place, reaction tubes one termination airing system; The other end connects mechanical pump, and keep-uping pressure is 200~300Torr (1Torr ≈ 133Pa), and continuing simultaneously to feed flow is the argon gas of 50~100sccm; Control reaction tubes central authorities temperature is 800 ℃ in the experiment, behind the insulation 4h, closes heating power supply; Naturally cool to room temperature, obtain yellow lint shape material.The sign of product utilization X-ray powder diffraction, sem (SEM) and photoluminescence spectrum (PL), electronic transport photoelectric properties test analysis, the product of preparation is the CdS nano wire, presents p type electroconductibility, promptly prepares p type CdS nano wire.There is not notable difference with structure, pattern and the photoelectric properties of CdS among embodiment 1 and the embodiment 2.
Above instance has proved at pressure condition in 200~300Torr scope; Carrier gas flux is in 50~100sccm scope; Stove heart temperature is in 800~900oC scope; P type CdS nano wire can prepare with the method in one's power in the above-mentioned instance, and structure, pattern and photoelectricity performance do not have considerable change.

Claims (2)

1. the preparation method of a p type CdS nano wire comprises:
(1) with CdS powder and Sn powder by mass ratio 2~4: 1 mixes and places on the aluminium sesquioxide boat of tube furnace, is substrate with p type silicon substrate, puts into the aluminium sesquioxide boat of starting material leeward;
(2) continuing to vacuumize the control furnace pressure is 200~300Torr, feeds the argon gas that flow is 50~100sccm simultaneously;
(3) control reaction tubes central authorities temperature is 800~900 ℃, behind insulation 2~4h, naturally cools to room temperature, promptly gets.
2. the preparation method of a kind of p type CdS nano wire according to claim 1; It is characterized in that: said p type silicon substrate is (100) face, and the surface is coated with the golden film of thickness for
Figure FDA0000135531810000011
.
CN2010105554956A 2010-11-23 2010-11-23 Method for preparing p-type CdS nanowires Expired - Fee Related CN101979723B (en)

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Publication number Priority date Publication date Assignee Title
CN102618269B (en) * 2012-03-13 2016-06-29 浙江理工大学 A kind of preparation method of CdS/Sn heterogeneous structural nano luminescent material
CN104213197B (en) * 2014-09-24 2017-06-16 中国电子科技集团公司第四十六研究所 A kind of doping method in situ that semiconductor single crystal material is prepared for PVT methods
CN107195722A (en) * 2017-07-12 2017-09-22 中国科学院上海技术物理研究所 A kind of distinguishable detector of room temperature nano wire number of photons and preparation method
CN107930623B (en) * 2017-11-16 2020-11-13 皖南医学院 Gold-urea complex nanosphere and preparation method thereof, and preparation method and application of porous nanogold
CN110047973B (en) * 2019-04-23 2020-05-01 范佳旭 Photoelectric sensor based on copper-doped cadmium sulfide nanowire and preparation method thereof
CN114497248A (en) * 2021-12-08 2022-05-13 华南师范大学 Photoelectric detector based on mixed-dimensional Sn-CdS/molybdenum telluride heterojunction and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101397149A (en) * 2008-10-23 2009-04-01 新疆大学 CdS nano rod growth method by catalyst-assisted and vacuum heat evaporation
KR20100089413A (en) * 2009-02-03 2010-08-12 고려대학교 산학협력단 Method of manufacturing solar cell substrate with cds/meh-ppv hybrid structure
CN101874286A (en) * 2007-11-27 2010-10-27 纳米晶公司 Ultra-low dislocation density Group III - Nitride semiconductor substrates grown via nano-or micro-particle film

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101874286A (en) * 2007-11-27 2010-10-27 纳米晶公司 Ultra-low dislocation density Group III - Nitride semiconductor substrates grown via nano-or micro-particle film
CN101397149A (en) * 2008-10-23 2009-04-01 新疆大学 CdS nano rod growth method by catalyst-assisted and vacuum heat evaporation
KR20100089413A (en) * 2009-02-03 2010-08-12 고려대학교 산학협력단 Method of manufacturing solar cell substrate with cds/meh-ppv hybrid structure

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