CN104952703A - Production method of IIB-VIB semiconductor/CdS nano P-N junction - Google Patents
Production method of IIB-VIB semiconductor/CdS nano P-N junction Download PDFInfo
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- CN104952703A CN104952703A CN201510257498.4A CN201510257498A CN104952703A CN 104952703 A CN104952703 A CN 104952703A CN 201510257498 A CN201510257498 A CN 201510257498A CN 104952703 A CN104952703 A CN 104952703A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02551—Group 12/16 materials
- H01L21/02557—Sulfides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02551—Group 12/16 materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02587—Structure
- H01L21/0259—Microstructure
- H01L21/02603—Nanowires
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD
Abstract
The invention discloses a nanomaterial and a production method of devices and particularly relates to a production method of an IIB-VIB semiconductor/CdS nano P-N junction. Based on a phosphor-doped P-type IIB-VIB semiconductor nanowire synthesized by chemical vapor deposition, the phosphor-doped P-type IIB-VIB semiconductor nanowire is coated with a grown CdS shell layer by means of atomic layer deposition; a gold electrode and a titanium electrode are produced on an IIB-VIB semiconductor/CdS core-shell structure by means of photoetching and electron beam evaporation; thus, a nano P-N junction device in the IIB-VIB semiconductor/CdS core-shell structure is produced. The nano P-N junction of the IIB-VIB semiconductor/CdS core-shell structure is good in performance, high in controllability and available for large-scale production; the production method is widely applicable to the field of nano optoelectronics, such as solar cells and photoelectric detection.
Description
Technical field
The present invention relates to a kind of nano material and device preparation method, relate in particular to the preparation method of a kind of IIB-VIB race semiconductor/CdS nanometer p-n junction.
Background technology
P-n junction is the core of modern photoelectron technology, and the many opto-electronic devices comprising photodetector, solar cell, light-emitting diode, imaging display etc. are all construct to form based on p-n junction.Therefore, to the research of opto-electronic device, be unable to do without constructing and applying of p-n junction.In the last few years, the research based on the nanometer p-n junction of various material system made great progress, and low dimension semiconductor nanometer p-n junction mainly comprises nucleocapsid structure (radial direction), axial arrangement, chi structure etc.And core-shell nano p-n junction is widely used in nano photovoltaic device and photoelectric detector due to advantages such as its interface area are large, the interface of such as its atomically flating nanometer p-n junction is possessed high photoelectric conversion efficiency etc.C. M. professor Lieber of Harvard University just confirms that silicon nanowires nucleocapsid structure has excellent photovoltaic performance (B. Tian, X. Zheng, T. J. Kempa, Y. Fang, N. Yu, G. Yu, J. Huang, C. M. Lieber, " Coaxial silicon nanowires as solar cells and nanoelectronic power sources "
nature449,885 (2007)).
The method preparing nuclear shell structure nano p-n junction at present mainly contains vapor growth method, thermal evaporation, solwution method etc.Such as HeFei University of Technology take off the people such as Jian Sheng professor invented a kind of method of chemical vapour deposition (CVD) one-step synthesis method Si/IIB-VIB race semiconductor nanowires p-n junction (method of a kind of one-step synthesis method Si/IIB-VIB race semiconductor nanowires p-n junction that utilizes, take off Jian Sheng, Wang Li, Yu Yongqiang, Wu Chunyan, Peng Qiang, Lu Min, Ren Yongbin, 201110048502.8, CN 102176410 B); The quick grade of Physical Chemistry Technology Inst., Chinese Academy of Sciences Meng Xiang has been invented one and has been utilized thermal evaporation to prepare One-Dimensional ZnO/SnO
2preparation method (One-Dimensional ZnO/the SnO of nuclear shell structure nano heterojunction semiconductor material
2the preparation method of nuclear shell structure nano heterojunction semiconductor material, Meng Xiangmin, Huang Xing, 201210068382.2, CN 102618849 B); Professor Yang Peidong of Univ California-Berkeley have developed a kind of method of carrying out cation exchange in the solution and prepares CdS/Cu
2the method of S nanowire core shell structure, and high performance nano solar battery (the Solution-processed core-shell nanowires for efficient photovoltaic cells that utilized this nucleocapsid structure to prepare, Jinyao Tang, ZiyangHuo, Sarah Brittman, Hanwei Gao and Peidong Yang, Nature Nanotechnology, 2011,6,9,568-572).Although said method has prepared the nuclear shell structure nano p-n junction of function admirable, their preparation process is complicated, and controllability is low, and is difficult to realize large-scale evenly preparation.
Summary of the invention
The present invention is directed to the deficiencies in the prior art part, aim to provide a kind of IIB-VIB race semiconductor/CdS nanometer p-n junction preparation method.IIB-VIB race semiconductor obtained by invention/CdS nuclear shell structure nano p-n junction is functional, controllability is high, can prepare on a large scale; The sub-field of the nano photoelectric such as solar cell, photodetection can be widely used in.
Technical solution problem of the present invention adopts following technological means:
The preparation method of a kind of IIB-VIB race semiconductor/CdS nanometer p-n junction, is characterized in that comprising the following steps:
Step 1: by using the phosphorus doping p-type IIB-VIB race semiconducting nanowires grow substrate of chemical gaseous phase depositing process synthesis to be directly positioned in the reaction chamber of ald, vacuumize, and heating makes cavity inner temperature remain 140-160 DEG C;
Step 2: with H
3cCSNH
2(thioacetamide) powder and liquid Cd (CH
3)
2(dimethyl cadmium) is presoma, and uses heating collar by H
3cCSNH
2be heated to 115-125 DEG C, nitrogen buffer gas and purified gas: first pass into H
3cCSNH
2presoma, forms first individual layer of S on p-type IIB-VIB race semiconductor nanowires surface; Then extract remaining presoma and nitrogen by mechanical pump after passing into nitrogen wash; Pass into Cd (CH again
3)
2, the first individual layer mentioned above is formed second individual layer of Cd, and the first individual layer and the second individual layer form S-Cd key; Extract remaining presoma and nitrogen by mechanical pump after passing into nitrogen wash, this is a circulation, and this cyclic process can at the CdS shell of a p-type IIB-VIB race semiconductor nanowires surface parcel unit; Repeat above-mentioned circulation, form CdS film on p-type IIB-VIB race semiconductor nanowires surface.
Step 3: be dispersed in organic solvent by prepared IIB-VIB race semiconductor/CdS nucleocapsid structure, adopts drop-coating to be transferred to by IIB-VIB race semiconductor/CdS nucleocapsid structure and prepares on substrate;
Step 4: preparing after substrate surface smears photoresist in step 3 is positioned in mask aligner, by to expose and development makes IIB-VIB race semiconductor/CdS nucleocapsid structure one end exposed, again this substrate is positioned in electron beam plated film instrument at CdS layer outside deposition Ti electrode, finally described substrate of preparing is positioned in acetone solvent, photoresist is decomposed, and obtains the IIB-VIB race semiconductor/CdS nucleocapsid structure of one end titanizing electrode;
Step 5: be again positioned in mask aligner preparing after substrate surface smears photoresist, by expose and development makes one end of IIB-VIB race semiconductor/CdS nucleocapsid structure plating Ti electrode cover photoresist, the other end is exposed; Then sample is positioned over the dilute hydrochloric acid solution immersion etching that mass ratio is 5%, passes through chemical reaction:
CdS + 2HCl = H
2S + CdCl
2
Etch away the CdS shell of IIB-VIB race semiconductor/exposed one end of CdS nucleocapsid structure, make p-type IIB-VIB race semiconductor nano line core exposed, finally the mode repeated in step 3 uses mask aligner and electron beam plated film instrument at exposed p-type IIB-VIB race's semiconductor side deposition Au electrode;
Step 6: prepared, obtains electroded IIB-VIB race semiconductor/CdS nuclear shell structure nano p-n junction device.
Preferred: the cavity inner temperature in step 1 remains 150 DEG C; Use heating collar by H in step 2
3cCSNH
2be heated to 120 DEG C.
Preferred: nitrogen flow is 10-20sccm, nitrogen gas purity >=99.9%.
Preferred: cycle-index is 300-600 circulation.
Preferred: described organic solvent is ethanol or isopropyl alcohol.
Preferred: the thickness of described Ti electrode and gold electrode is 50nm.
Preferred: etch period is 180-360S.
Preferred: described substrate of preparing is sapphire, oxidized silicon chip or quartz glass.
Preferred: described IIB-VIB race semiconductor nanowires is ZnSe, ZnS, ZnTe, CdSe, CdS or CdTe.
Beneficial effect of the present invention is: utilize Atomic layer deposition method at p-type IIB-VIB race semiconductor nanowires surface deposition CdS shell, the synthesis of nanometer nuclear shell nano-structure accurately can be controlled in atomic level, make that synthesized nanometer p-n junction interface is sharp-pointed, defect is few, is beneficial to the opto-electronic conversion in optoelectronic device applications.Use nitrogen gas purity >=99.9%, effectively can ensure that the chemical reaction in reaction chamber is more abundant, impurity is less.Cycle-index is 300-600 circulation, and CdS layer deposit thickness can be made to reach 20-40 nm, and this process control is high, can realize extensive preparation.The thickness of Ti electrode and gold electrode is 50 nm, the p-n junction that preparation can be made to complete reaches and uses normal use standard (Surface induced negative photoconductivity i n p-type ZnSe: B i nanowires and their nano-optoelectronic applications, Xiwei Zhang, Jiansheng Jie, Zhi Wang, Chunyan Wu, Li Wang, Qiang Peng, Yongqiang Yu, Peng Jiang and Chao Xie, J. Mater. Chem., 2011,21,6736).Etch period is 180-360 S, and mass ratio 5% watery hydrochloric acid and CdS shell can be made to reflect more abundant.Substrate prepared by device is sapphire, oxidized silicon chip or quartz glass, and make chemical reaction more stable, impurity is less.
Above-mentioned explanation is only the general introduction of technical solution of the present invention, in order to can clearer understanding technological means of the present invention, and can be implemented according to description, below coordinates accompanying drawing to be described in detail as follows for preferred embodiments of the present invention.The specific embodiment of the present invention is provided in detail by following examples and accompanying drawing thereof.
Accompanying drawing explanation
Fig. 1 is ZnSe/CdS nanometer nuclear shell nano-structure ESEM schematic diagram prepared by sublayer, embodiment 1 Central Plains sedimentation.
Fig. 2 is the energy spectrogram of ZnSe/CdS nanometer nuclear shell nano-structure prepared in embodiment 1.
Fig. 3 is the transmission electron microscope figure of ZnSe/CdS nanometer nuclear shell nano-structure prepared in embodiment 1.
Fig. 4 is the X ray diffracting spectrum of ZnSe/CdS nanometer nuclear shell nano-structure prepared in embodiment 1.
Fig. 5 is the device schematic top plan view in embodiment 1 after one end of prepared ZnSe/CdS nucleocapsid structure deposits 50 nm Ti electrode.
Fig. 6 completes second time photoetching and utilizes photoresist protective layer to protect the device schematic top plan view behind Ti electrode one end in embodiment 1.
Fig. 7 completes dilute hydrochloric acid solution to soak the device schematic top plan view after etching in embodiment 1.
Fig. 8 completes third time photoetching and the device schematic top plan view of electron beam plated film after exposed ZnSe core one end deposits 50 nm gold electrodes in embodiment 1.
Fig. 9 is ZnSe/CdS nuclear shell structure nano p-n junction device scanning electron microscope diagram prepared in embodiment 1.
Figure 10 is ZnSe/CdS nuclear shell structure nano p-n junction Device current-voltage curve synoptic diagram prepared in embodiment 1.
Sequence number in figure: 1: substrate prepared by device, 2:ZnSe/CdS nucleocapsid structure, 3:CdS shell, 4:Ti electrode, 5: photoresist protective layer, 6:Au electrode.
Specific embodiment
Embodiment selects p-type ZnSe nano wire to be p-type IIB-VIB race semiconductor nanowires.Specifically describe as follows:
Embodiment 1:
By using the phosphorus doping p-type ZnSe Nanowire growth substrate of chemical gaseous phase depositing process synthesis to be directly positioned in the reaction chamber of ald, vacuumizing, reaction chamber heated and makes cavity inner temperature remain 150 DEG C; With H
3cCSNH
2powder and liquid Cd (CH
3)
2for presoma provides S source and Cd source respectively, use heating collar to H
3cCSNH
2presoma is heated to 120 DEG C; Nitrogen buffer gas and purified gas; Flow control is 20sccm, first passes into H
3cCSNH
2, the time of passing into is 0.015S, extracts remaining presoma and nitrogen after passing into nitrogen wash 10S by mechanical pump; Pass into Cd (CH again
3)
2the time of passing into is 0.015S, and extract remaining presoma nitrogen by mechanical pump after passing into nitrogen wash 10S, after two kinds of precursors reach ZnSe nanowire surface, their are understood at its chemical absorption of surface and surface reaction occurs, thus adventitious deposit, this is a circulation; After 450 circulations, be the CdS shell of 30nm thickness at p-type ZnSe nano wire top layer parcel growth thickness.
As shown in Figure 1, can observe and deposited thin film at p-type ZnSe surface uniform.
As shown in Figure 2, ESEM power dissipation energy spectrogram can confirm that sample comprises Zn, Se, Cd, S tetra-kinds of elements.
As shown in Figure 3, transmission electron microscope figure shows that this structure is the nucleocapsid structure of one dimension.
As shown in Figure 4, X ray diffracting spectrum confirms that this nucleocapsid structure has the good ZnSe phase of crystal mass and CdS phase.
As shown in Figure 5-Figure 8, prepared ZnSe/CdS nucleocapsid structure solwution method split-up is prepared on substrate 1 to device, shown by first time photoetching and electron beam plated film deposit 50 nm Ti electrodes 4 at the CdS shell 3 of prepared ZnSe/CdS nucleocapsid structure 2; By second time photoetching, photoresist protective layer 5 is utilized to protect Ti electrode one end; Then sample being positioned over mass ratio is soak etching 270S in the dilute hydrochloric acid solution of 5%, by chemical reaction etching CdS shell, makes ZnSe core exposed; Deposit the Au electrode 6 of 50 nm by third time photoetching and electron beam plated film in one end of exposed ZnSe core, thus prepare ZnSe/CdS nuclear shell structure nano p-n junction device.
As shown in Figure 9, the ZnSe/CdS nuclear shell structure nano p-n junction scanning electron microscope diagram prepared by the present embodiment, nucleocapsid structure is obvious as can be observed from Figure.
As shown in Figure 10, its electrical characterization be shown with good rectification characteristic, meet the feature of p-n junction, its commutating ratio when ± 3V reaches 30.
Embodiment 2:
By using the phosphorus doping p-type ZnSe Nanowire growth substrate of chemical gaseous phase depositing process synthesis to be directly positioned in the reaction chamber of ald, vacuumize, heating reaction chamber also makes cavity inner temperature remain 150 DEG C; With H
3cCSNH
2with Cd (CH
3)
2there is provided S source and Cd source for presoma is respectively reaction, and use heating collar by H
3cCSNH
2presoma is heated to 120 DEG C; Nitrogen buffer gas and purified gas: flow control is 20sccm, first passes into H
3cCSNH
2, the time of passing into is 0.015S, extracts remaining presoma and nitrogen, then pass into Cd (CH after passing into nitrogen wash 10S by mechanical pump
3)
2, the time of passing into is 0.015S, extracts remaining presoma nitrogen after passing into nitrogen wash 10S by mechanical pump, and when two kinds of precursors reach ZnSe nanowire surface, their are understood at its chemical absorption of surface and surface reaction occurs, thus adventitious deposit, this is a circulation; After 300 circulations, be the CdS shell of 20nm thickness at p-type ZnSe nano wire top layer parcel growth thickness.
Prepared ZnSe/CdS nucleocapsid structure solwution method split-up is prepared on substrate to device, shown in by first time photoetching and electron beam plated film at the side of prepared nucleocapsid structure deposition 50nm Ti electrode, by second time photoetching, photoresist is utilized to do mask protection Ti electrode side, then sample is positioned over the dilute hydrochloric acid solution immersion etching 180S that mass ratio is 5%, remove CdS shell by chemical reaction, make ZnSe core exposed; By third time photoetching and the electron beam plated film gold electrode at the side of exposed ZnSe deposition 50nm, thus prepare ZnSe/CdS nuclear shell structure nano p-n junction device.
Although the present invention with preferred embodiment openly as above; so it is not intended to limiting the invention; anyly have the knack of this those skilled in the art; without departing from the spirit and scope of the present invention make an amendment, change and retouching, the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.
Claims (9)
1. a preparation method for IIB-VIB race semiconductor/CdS nanometer p-n junction, is characterized in that comprising the following steps:
Step 1: by using the phosphorus doping p-type IIB-VIB race semiconducting nanowires grow substrate of chemical gaseous phase depositing process synthesis to be directly positioned in the reaction chamber of ald, vacuumize, and heating makes cavity inner temperature remain 140-160 DEG C;
Step 2: with H
3cCSNH
2powder and liquid Cd (CH
3)
2for presoma, and use heating collar that H3CCSNH2 powder is heated to 115-125 DEG C, nitrogen buffer gas and purified gas: first pass into H3CCSNH2 presoma, form first individual layer of S on p-type IIB-VIB race semiconductor nanowires surface; Then extract remaining presoma and nitrogen by mechanical pump after passing into nitrogen wash; Logical Cd (CH again
3)
2, the first individual layer mentioned above is formed second individual layer of Cd, and the first individual layer and the second individual layer form S-Cd key; Extract remaining presoma and nitrogen by mechanical pump after passing into nitrogen wash, this is a circulation, and this cyclic process can at the CdS shell of a p-type IIB-VIB race semiconductor nanowires surface parcel unit; Repeat above-mentioned circulation, form CdS film on p-type IIB-VIB race semiconductor nanowires surface;
Step 3: be dispersed in organic solvent by prepared IIB-VIB race semiconductor/CdS nucleocapsid structure, adopts drop-coating to be transferred to by IIB-VIB race semiconductor/CdS nucleocapsid structure and prepares on substrate;
Step 4: preparing after substrate surface smears photoresist in step 3 is positioned in mask aligner, by to expose and development makes IIB-VIB race semiconductor/CdS nucleocapsid structure one end exposed, again this substrate is positioned in electron beam plated film instrument at CdS layer outside deposition Ti electrode, finally described substrate of preparing is positioned in acetone solvent, photoresist is decomposed, and obtains the IIB-VIB race semiconductor/CdS nucleocapsid structure of one end titanizing electrode;
Step 5: be again positioned in mask aligner preparing after substrate surface smears photoresist, by expose and development makes one end of IIB-VIB race semiconductor/CdS nucleocapsid structure titanizing electrode cover photoresist, the other end is exposed; Then sample is positioned over the dilute hydrochloric acid solution immersion etching that mass ratio is 5%, passes through chemical reaction:
CdS + 2HCl = H
2S + CdCl
2
Etch away the CdS shell of IIB-VIB race semiconductor/exposed one end of CdS nucleocapsid structure, make p-type IIB-VIB race semiconductor nano line core exposed, finally the mode repeated in step 3 uses mask aligner and electron beam plated film instrument at the side deposited gold electrode of exposed p-type IIB-VIB race semiconductor nanowires;
Step 6: prepared, obtains electroded IIB-VIB race semiconductor/CdS nuclear shell structure nano p-n junction device.
2. the preparation method of IIB-VIB race according to claim 1 semiconductor/CdS nanometer p-n junction, is characterized in that the cavity inner temperature in step 1 remains 150 DEG C; Use heating collar that H3CCSNH2 is heated to 120 DEG C in step 2.
3. the preparation method of IIB-VIB race according to claim 1 semiconductor/CdS nanometer p-n junction, is characterized in that: nitrogen flow is 10-20sccm, nitrogen gas purity >=99.9%.
4. the preparation method of IIB-VIB race according to claim 1 semiconductor/CdS nanometer p-n junction, is characterized in that: cycle-index is 300-600 circulation.
5. the preparation method of IIB-VIB race according to claim 1 semiconductor/CdS nanometer p-n junction, is characterized in that described organic solvent is ethanol or isopropyl alcohol.
6. the preparation method of IIB-VIB race according to claim 1 semiconductor/CdS nanometer p-n junction, is characterized in that: the thickness of described Ti electrode and gold electrode is 50nm.
7. the preparation method of IIB-VIB race according to claim 1 semiconductor/CdS nanometer p-n junction, is characterized in that: etch period is 180-360S.
8. the preparation method of IIB-VIB race according to claim 1 semiconductor/CdS nanometer p-n junction, is characterized in that: described substrate of preparing is sapphire, oxidized silicon chip or quartz glass.
9. the preparation method of IIB-VIB race as claimed in any of claims 1 to 8 semiconductor/CdS nanometer p-n junction, is characterized in that: described IIB-VIB race semiconductor is ZnSe, ZnS, ZnTe, CdSe, CdS or CdTe.
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| CN108400178A (en) * | 2018-04-27 | 2018-08-14 | 安阳师范学院 | A kind of folded nano wire film solar cell of the cross arrangement layer heap of interlayer component alternation |
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| CN106057931A (en) * | 2016-07-05 | 2016-10-26 | 安阳师范学院 | Large open-circuit voltage nano heterojunction solar energy cell and manufacturing method |
| CN108400178A (en) * | 2018-04-27 | 2018-08-14 | 安阳师范学院 | A kind of folded nano wire film solar cell of the cross arrangement layer heap of interlayer component alternation |
| CN108400178B (en) * | 2018-04-27 | 2023-08-25 | 安阳师范学院 | Cross-arrangement layer stacked nanowire thin film solar cell with graded interlayer components |
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