CN100544040C - The treatment process of cadmium telluride material surface oxidation film - Google Patents
The treatment process of cadmium telluride material surface oxidation film Download PDFInfo
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- CN100544040C CN100544040C CNB2007100402851A CN200710040285A CN100544040C CN 100544040 C CN100544040 C CN 100544040C CN B2007100402851 A CNB2007100402851 A CN B2007100402851A CN 200710040285 A CN200710040285 A CN 200710040285A CN 100544040 C CN100544040 C CN 100544040C
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- cadmium telluride
- telluride material
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Abstract
The treatment process of cadmium telluride material surface oxidation film, be earlier with after acetone, absolute ethyl alcohol, the washed with de-ionized water with the cadmium telluride material, through bromine and ethanol solution corrosion, carry out surface treatment with lactic acid and ethylene glycol solution again, can obtain the few even oxide-free cadmium telluride surface of oxide.Can improve photoelectric properties, rate of finished products and the reliability of cadmium telluride photovoltaic detector array greatly, whole technical process is simple, and is easy to operate, and good reproducibility is practical, and human body is not had injury substantially.Can be widely used in the preparation of cadmium telluride material surface and the manufacturing of cadmium telluride photoelectric device.
Description
Technical field
The present invention relates to the treatment process of cadmium telluride material surface oxidation film, be specifically related to adopt Bridgman method, metal organic-matter chemical vapor deposition method, and the treatment process of the cadmium telluride material surface oxidation film of molecular beam epitaxial method growth, this technology is mainly used in optoelectronic areas such as photoelectron material and photodetector.
Background technology
The physical characteristic of wide band gap semiconducter and the research of chemical characteristic remain challenging problem in photovoltaic technology.In this based semiconductor, the most representative with the II-VI compounds of group.Silicon in IV family material is the same with GaAs in the III-V compounds of group, and CdTe is the important materials in the II-VI compounds of group, and CdTe has n type and two kinds of conduction types of p type, and two kinds of mobility of charge carrier rates are all better.At present, CdTe has been widely used for preparing various photo-detectors.Because the CdTe film has the direct band gap structure, its absorption coefficient of light (to the light of wavelength less than ABSORPTION EDGE) is very big; Thickness is the film of 1 μ m, is enough to absorb greater than 99% of the emittance of CdTe forbidden band energy, has therefore reduced the requirement to diffuse length, makes it become the optimal material of preparation efficient solar battery.Because the cadmium telluride material has character such as superior optics, magnetics, electricity, thereby is widely used in the photoelectric device, especially is applied to High Performance X-ray and Detection of Space Particles Radiation device.Therefore, how to prepare the plane of crystal that satisfies the High Performance X-ray request detector effectively, be the problem that the researcher explores for many years always.In the manufacturing process of Cd Te probe, require the in addition strict control of the surface of this wide bandgap semiconductor materials, make the surface have uniform stoicheiometry, no crystal defect, few surface oxidation and other surface contaminations.In addition, being etched in the making CdTe/CdS battery is one of crucial technology, has the etching solution of report to have: Br
2-methyl alcohol, HNO
3-H
3PO
4(NH) and K
2Cr
2O
7: H
2SO
4Deng.
Because cadmium telluride is the bianry alloy material, in process of surface treatment, be easy to cause the stoicheiometry uneven surfaces, as chemical segregation occurs and cause rich Te layer, even be easy to along the crystal boundary etching, also make the surface produce oxidation film layer and defective easily, finally be difficult to obtain stoicheiometry evenly and the smooth finish surface of non-oxidation.In with insulation or the passivation technology of semi-insulating medium as passivation layer, the surface oxide layer of cadmium telluride not only influences interfacial characteristics, and directly has influence on the dielectric property of passivation layer, finally influences photoelectric properties, rate of finished products, the reliability of detector array.Usually adopt bromine and methanol solution to carry out surface treatment at present, but make the surface produce " segregation " problem easily.Simultaneously, methyl alcohol is bigger to people's eyes infringement, and long-term contact will cause eyes blind.For this reason, the researcher seeks for many years always and can prepare the surface treatment method that satisfies the requirement of high-performance Infrared Detectors effectively.People have carried out exploring and research (Aramoto T, et., J.Appl.Phys., 1997,36 (10), 6304 to different cadmium telluride surface treatment methods; K.Durose, et., J.Appl.Phys., 1993,73,8381), but do not find a kind of comparatively desirable processing method yet.
Summary of the invention
The surface oxidation film treatment process that the purpose of this invention is to provide a kind of cadmium telluride material, overcoming existing treatment process causes the surface chemistry proportioning inhomogeneous easily, even be easy to along the crystal boundary etching, especially the cadmium telluride material is used to make photoelectric device, existing treatment process directly has influence on the dielectric property of passivation layer, make photoelectric properties, rate of finished products, the reliability extreme difference of detector array, be difficult to obtain stoicheiometry evenly and the smooth finish surface of non-oxidation, and very big to the human injury; The cadmium telluride material that uses the inventive method to handle not only has the surface of uniform stoicheiometry, bright and clean, no crystal defect, and has a few even oxide-free cadmium telluride surface of oxide, highly beneficial to the photoelectric properties, rate of finished products, the reliability that improve cadmium telluride photovoltaic detector array, whole technical process is simple, easy to operate, practical, and human body do not had injury substantially.
The treatment process of cadmium telluride material surface oxidation film comprises the cadmium telluride material is carried out clean; Corrosion treatment and surface treatment; It is characterized in that:
A), earlier the cadmium telluride material is carried out clean:
A, in acetone soln, soaked 2～3 minutes;
B, in absolute ethyl alcohol, soaked 1～2 minute;
Cleaned 1～2 minute in c, the deionized water at room temperature;
D, dry up with high pure nitrogen (99%).
B), again the cadmium telluride material is carried out corrosion treatment:
A, with the cadmium telluride material that dries up with bromine and ethanol solution corrosion, the volume ratio of bromine and ethanol solution is (0.005～0.1): 1, etching time is 10～60 seconds, and ceaselessly rocks the cadmium telluride material in corrosion process;
B, in absolute ethyl alcohol, cleaned 1～2 minute.
C), at last the cadmium telluride material is carried out surface treatment:
A, the cadmium telluride material is immersed lactic acid and ethylene glycol solution, the volume ratio of lactic acid and ethylene glycol solution is (0.03～0.1): 1, in solution, soaked 1～2 minute;
B, subsequently the cadmium telluride material was cleaned 1～2 minute with absolute ethyl alcohol;
C, washed 1～2 minute with washed with de-ionized water again;
D, use high pure nitrogen (99%) to dry up at last.
Use the treatment process of cadmium telluride material surface oxidation film of the present invention, reduce or remove the oxide on cadmium telluride surface, can improve photoelectric properties, rate of finished products and the reliability of cadmium telluride Photovoltaic Detector Array greatly by surface treatment.Particularly quality and the effect to improving the cadmium telluride surface passivation will play a key role.Whole technical process is simple, and is easy to operate, and good reproducibility is practical, and human body is not had injury substantially, can be widely used in the preparation of cadmium telluride material surface and the manufacturing of cadmium telluride photoelectric device.
Description of drawings
Fig. 1 is the photoelectron spectroscopy of the Te3d that gathered of cadmium telluride material surface that the present invention handles;
Fig. 2 is the photoelectron spectroscopy of the Cd3d that gathered of cadmium telluride material surface that the present invention handles;
Fig. 3 is the photoelectron spectroscopy of the O1s that gathered of cadmium telluride material surface that the present invention handles;
Te3d among Fig. 1
5/2Only have one unimodal, show the surface almost the tellurium of non-oxidation state occur.Cd3d among Fig. 2 spectrum analyzed draw, because the chemical shift of Cd is minimum, it is less to illustrate that the CdTe surface contains the oxide of Cd.In order to determine the chemical composition on surface, with Gaussian O1s is carried out match, the matched curve of O1s Gaussian only has a single peak position to exist, as shown in Figure 3.Matched curve overlaps fully with empirical curve, and the binding energy of peak position is 532.6eV, and it shows that corresponding to lip-deep oxygen physisorption (as hydrogen-oxygen or carbon-family of oxygen group) the surperficial oxide-free of cadmium telluride material exists in the detection limit scope.
Embodiment
Cadmium telluride (CdTe) material that following examples are selected is the monocrystal material that adopts vertical Bridgman method growth.Material is specifically implemented by method of the present invention and step after surperficial grinding and polishing, cleaning.
Embodiment 1
A, elder generation soaked in acetone soln 2～3 minutes, put into absolute ethyl alcohol again and soaked 1～2 minute, cleaned in the deionized water at room temperature 1～2 minute subsequently, dried up with high pure nitrogen (99%);
B, with the cadmium telluride material that dries up with bromine and ethanol solution corrosion, the volume ratio of bromine and ethanol solution is 0.005:1, etching time is 60 seconds, and ceaselessly rocks the cadmium telluride material in corrosion process; Be placed on then and clean 1～2 minute in the absolute ethyl alcohol;
C, the cadmium telluride material is immersed lactic acid and ethylene glycol solution immediately, the volume ratio of lactic acid and ethylene glycol solution is 0.03:1, in solution, soaked 2 minutes, subsequently the cadmium telluride material was cleaned 1～2 minute with absolute ethyl alcohol, use washed with de-ionized water again 1～2 minute, and used high pure nitrogen (99%) to dry up at last.
A, elder generation soaked in acetone soln 2～3 minutes, put into absolute ethyl alcohol again and soaked 1～2 minute, cleaned in the deionized water at room temperature 1～2 minute subsequently, dried up with high pure nitrogen (99%);
B, with the cadmium telluride material that dries up with bromine and ethanol solution corrosion, the volume ratio of bromine and ethanol solution is 0.01:1, etching time is 50 seconds, and ceaselessly rocks the cadmium telluride material in corrosion process; Be placed on then and clean 1～2 minute in the absolute ethyl alcohol;
C, the cadmium telluride material is immersed lactic acid and ethylene glycol solution immediately, the volume ratio of lactic acid and ethylene glycol solution is 0.05:1, in solution, soaked for 90 seconds, subsequently the cadmium telluride material was cleaned 1～2 minute with absolute ethyl alcohol, use washed with de-ionized water again 1～2 minute, and used high pure nitrogen (99%) to dry up at last.
Embodiment 3
A, elder generation soaked in acetone soln 2～3 minutes, put into absolute ethyl alcohol again and soaked 1～2 minute, cleaned in the deionized water at room temperature 1～2 minute subsequently, dried up with high pure nitrogen (99%);
B, with the cadmium telluride material that dries up with bromine and ethanol solution corrosion, the volume ratio of bromine and ethanol solution is 0.05:1, etching time is 30 seconds, and ceaselessly rocks the cadmium telluride material in corrosion process; Be placed on then and clean 1～2 minute in the absolute ethyl alcohol;
C, be about to the cadmium telluride material and immerse lactic acid and ethylene glycol solution, the volume ratio of lactic acid and ethylene glycol solution is 0.08:1, in solution, soaked for 70 seconds, subsequently the cadmium telluride material was cleaned 1～2 minute with absolute ethyl alcohol, washed 1～2 minute with washed with de-ionized water again, use high pure nitrogen (99%) to dry up at last.
Embodiment 4
A, elder generation soaked in acetone soln 2～3 minutes, put into absolute ethyl alcohol again and soaked 1～2 minute, cleaned in the deionized water at room temperature 1～2 minute subsequently, dried up with high pure nitrogen (99%);
B, with the cadmium telluride material that dries up with bromine and ethanol solution corrosion, the volume ratio of bromine and ethanol solution is 0.08:1, etching time is 30 seconds, and ceaselessly rocks the cadmium telluride material in corrosion process; Be placed on then and clean 1～2 minute in the absolute ethyl alcohol;
C, be about to the cadmium telluride material and immerse lactic acid and ethylene glycol solution, the volume ratio of lactic acid and ethylene glycol solution is 0.1:1, in solution, soaked 1 minute, subsequently the cadmium telluride material was cleaned 1～2 minute with absolute ethyl alcohol, washed 1～2 minute with washed with de-ionized water again, use high pure nitrogen (99%) to dry up at last.
Embodiment 5
A, elder generation soaked in acetone soln 2～3 minutes, put into absolute ethyl alcohol again and soaked 1～2 minute, cleaned in the deionized water at room temperature 1～2 minute subsequently, dried up with high pure nitrogen (99%);
B, with the cadmium telluride material that dries up with bromine and ethanol solution corrosion, the volume ratio of bromine and ethanol solution is 0.1:1, etching time is 10 seconds, and ceaselessly rocks the cadmium telluride material in corrosion process; Be placed on then and clean 1～2 minute in the absolute ethyl alcohol;
C, the cadmium telluride material is immersed lactic acid and ethylene glycol solution immediately, the volume ratio of lactic acid and ethylene glycol solution is 0.1:1, in solution, soaked 1 minute, subsequently the cadmium telluride material was cleaned 1～2 minute with absolute ethyl alcohol, washed 1～2 minute with washed with de-ionized water again, use high pure nitrogen (99%) to dry up at last.
Utilize x-ray photoelectron spectroscopy respectively measurement, analysis to be carried out in the cadmium telluride surface through above-mentioned PROCESS FOR TREATMENT.The result shows that in the detection limit scope, the surface of cadmium telluride material has only oxygen physisorption, and surperficial oxide-free exists, and further specifies and adopts treatment process of the present invention, can obtain the cadmium telluride surface of the few even non-oxidation of oxide.
Whole technical process is simple, and is easy to operate, and good reproducibility is practical, and human body is not had injury substantially, can be widely used in the preparation of cadmium telluride material surface and the manufacturing of cadmium telluride photoelectric device.
Claims (1)
1. the treatment process of cadmium telluride material surface oxidation film comprises the cadmium telluride material is carried out clean; Corrosion treatment and surface treatment; It is characterized in that:
A) earlier the cadmium telluride material is carried out clean:
A) in acetone soln, soak 2～3 minutes;
B) in absolute ethyl alcohol, soak 1～2 minute;
C) cleaned in the deionized water at room temperature 1～2 minute;
D) dry up with 99% high pure nitrogen;
B) again the cadmium telluride material is carried out corrosion treatment:
A) the cadmium telluride material that dries up is corroded with bromine and ethanol solution, the volume ratio of bromine and ethanol solution is (0.005～0.1): 1, and etching time is 10～60 seconds, and ceaselessly rocks the cadmium telluride material in corrosion process;
B) in absolute ethyl alcohol, clean 1～2 minute;
C) at last the cadmium telluride material is carried out surface treatment:
A) the cadmium telluride material is immersed lactic acid and ethylene glycol solution, the volume ratio of lactic acid and ethylene glycol solution is (0.03～0.1): 1, in solution, soaked 1～2 minute;
B) subsequently the cadmium telluride material was cleaned 1～2 minute with absolute ethyl alcohol;
C) used washed with de-ionized water again 1～2 minute;
D) dry up with 99% high pure nitrogen at last.
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| CN102468366A (en) * | 2010-11-18 | 2012-05-23 | 比亚迪股份有限公司 | Cadmium telluride solar battery and preparation method thereof |
| CN109019531B (en) * | 2018-08-07 | 2021-12-17 | 中船重工黄冈贵金属有限公司 | Method for preparing high-purity tellurium dioxide by taking crude tellurium as raw material |
| CN110021683A (en) * | 2019-03-07 | 2019-07-16 | 中山瑞科新能源有限公司 | A kind of cadmium telluride solar cell substrate treatment process |
| CN111312855B (en) * | 2020-02-24 | 2022-04-19 | 京东方科技集团股份有限公司 | Preparation method of photoelectric detector |
| CN112592719B (en) * | 2020-08-04 | 2022-06-28 | 中国电子科技集团公司第十一研究所 | Corrosive liquid and corrosion method for corroding cadmium telluride CdTe thin film on mercury cadmium telluride surface |
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Non-Patent Citations (4)
| Title |
|---|
| 液相外延碲镉汞薄膜表面氧化特性的光电子能谱研究. 李毅等.物理学报，第49卷第1期. 2000 |
| 液相外延碲镉汞薄膜表面氧化特性的光电子能谱研究. 李毅等.物理学报，第49卷第1期. 2000 * |
| 碲镉汞表面氧化特性的光电子能谱研究. 李毅等.半导体学报，第18卷第12期. 1997 |
| 碲镉汞表面氧化特性的光电子能谱研究. 李毅等.半导体学报，第18卷第12期. 1997 * |
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