CN103074677A - Preparation method for zinc telluride homoepitaxy layer - Google Patents
Preparation method for zinc telluride homoepitaxy layer Download PDFInfo
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Abstract
The invention discloses a preparation method for a zinc telluride (ZnTe) homoepitaxy layer and belongs to the technical field of semiconductor materials. The preparation method comprises the steps as follows: adopting a low-pressure metal organic chemical vapor phase epitaxy process, taking dimethyl zinc and diethyl telluride as metal organic sources and hydrogen gas as carrier gas, and growing the ZnTe homoepitaxy layer on a ZnTe (100) substrate by low-pressure metal organic chemical vapor phase epitaxy equipment. The ZnTe homoepitaxy layer prepared with the method is narrow in band edge exciton peak and XRC (X-ray diffraction rocking curve) half-width, deep energy level emission of oxygen bound excitons, dislocation-related Y rays and the like does not appear, and the results show that the epitaxial layer is very good in crystal quality. The ZnTe homoepitaxy layer prepared with the method can be used for manufacturing photoelectric devices such as green LEDs and LDs, terahertz emitters and the like, and has a wide application prospect.
Description
Technical field
The present invention relates to a kind of preparation method of zinc telluridse homogeneity epitaxial layer, particularly a kind of method for preparing high quality zinc telluridse homogeneity epitaxial layer by control growth temperature and growth air pressure.
Background technology
Zinc telluridse (ZnTe) is a kind of important II-IV group iii v compound semiconductor material.ZnTe is direct band gap, and energy gap is 2.26eV under the room temperature, therefore in the photoelectric devices such as green light LED, terahertz detector, solar cell and optical waveguides good application prospect is arranged.At present, successfully utilize the aluminium diffusion technique to prepare room temperature luminous wavelength and be the ZnTe photodiode (LED) of 550nm.The preparation method who establishes high quality ZnTe epitaxial film has vital effect to producing efficient LED and laser diode (LD).Metal organic chemical vapor deposition (MOVPE) technique is the epitaxy technology that is widely adopted at present owing to have the epitaxial film good uniformity and be suitable for the advantage such as scale operation.Yet, some are comprised the photoelectric device (such as LED and LD etc.) of low dimensional structures (such as quantum well and quantum dot), need in process of growth, accurately control outer layer growth speed, this growing technology to epitaxial film is had higher requirement.
Simultaneously, there are the following problems usually for the zinc telluridse homogeneity epitaxial layer of normal pressure MOVPE growth:
1, in the outer layer growth process, the impurity atoms diffusion (out-diffusion) in the substrate can affect the quality of epitaxial film to epitaxial film.
2, the volatile impunty that derives from substrate mixes epitaxial film and causes auto-doping in process of growth, can cause the decline of epitaxial layer quality.
3, in the epitaxial process harmful parasitic reaction and gas-phase nucleation can appear.
4, the oxide compound of substrate surface can form the oxygen bound exciton in epitaxial film, and this class deep level emission can affect the luminescent properties of ZnTe epitaxial film.
5, the deep level emission (Y line) that caused by dislocation can appear in the ZnTe epitaxial film of normal pressure MOVPE growth usually.
Document " growth and the optical characteristics of the zinc telluridse homogeneity epitaxial layer of MOCVD method growth " (see academic journal " Journal of Crystal Growth ", 2003, the 248th volume, the 43rd page.) a kind of APMOCVD method of using is disclosed in the method for growth zinc telluridse iso-epitaxy film, namely there are the luminous compositions of deep energy level such as Y line and oxygen bound exciton in the zinc telluridse iso-epitaxy film of the method preparation, and this can affect its application in luminescent device.
Summary of the invention
For the problem that exists in the zinc telluridse homogeneity epitaxial layer preparation process, the invention provides a kind of preparation method of high quality zinc telluridse homogeneity epitaxial layer.
Technical scheme of the present invention realizes in the following manner:
A kind of preparation method of zinc telluridse homogeneity epitaxial layer, adopt low pressure MOVPE technique, take zinc methide and tellurium diethyl as metal organic source, with hydrogen as carrier gas, with low pressure metal organic chemistry vapour phase epitaxy equipment at ZnTe(100) Grown zinc telluridse epitaxial film; Its processing condition are as follows:
Chamber pressure: 100-760Torr;
Underlayer temperature during growth: 380-460 ° C;
Zinc methide transports speed: 10-30 μ mol/min;
Tellurium diethyl transports speed: 10-30 μ mol/min;
Growth time: 2-10 hour;
Above-mentioned preparation method's operation steps is as follows:
1, the cleaning of ZnTe substrate: (100) face ZnTe substrate in organic solvent-acetone after ultrasonic cleaning 3-5 minute, is put in the 1% bromine methanol solution at immersion treatment 20-30 minute, rinses well with deionized water at last;
2, the MOVPE equipment reaction chamber is passed into H
2, kept 20-40 minute at 500-600 ° of C, remove the oxide compound of ZnTe substrate surface;
3, underlayer temperature is controlled at 380-460 ° of C, regulate hydrogen flowing quantity, make zinc methide (DMZn) and tellurium diethyl (DETe) transport speed and all maintain 10-30 μ mol/min, control chamber pressure at 100-760Torr, growth time 2-10 hour;
4, growth finishes, and closes zinc source and tellurium source, and the stopped heating substrate is at ZnTe(100) Grown goes out the ZnTe epitaxial film, continues to pass into hydrogen 20-30 minute, is down to room temperature.
Preferred processing condition are as follows:
Underlayer temperature during growth: 400 ° of C;
Chamber pressure: 300Torr
Zinc methide transports speed: 15 μ mol/min;
Tellurium diethyl transports speed: 15 μ mol/min;
Growth time: 3 hours.
Preferably, described zinc methide purity is 99.9999%; Tellurium diethyl purity is 99.9999%.
Above-mentioned MOVPE equipment is low pressure metal organic chemistry vapour phase epitaxy equipment.
The inventive method has been owing to taked following measure in preparation epitaxial film process, thereby improved the crystalline quality of epitaxial film.
1, the DMZn of use high-purity (99.9999%) and DETe avoid reducing crystalline quality because introducing too much impurity as metal organic source.
2, heated substrate is removed oxide on surface in hydrogen, to avoid the occurring emission of oxygen bound exciton in the epitaxial film PL spectrum.
3, the speed that transports of keeping DMZn and DETe is 15 μ mol/min, makes ZnTe keep desirable stoicheiometry.
4, by reducing chamber pressure, can weaken the auto-doping from substrate, this is because the low reaction chamber pressure has increased the spread coefficient of the volatile impunty that is derived from substrate, and most of impurity is taken away by main air stream; On the other hand, reduce the thermograde that chamber pressure has increased substrate surface, reduced the thickness of the high temperature reaction zone of substrate surface, thereby suppressed harmful parasitic reaction and gas-phase nucleation.Therefore, the low reaction chamber pressure can improve the crystalline quality of epitaxial film.
5, improve its crystalline quality by the Optimal Growing temperature.Improve growth temperature and can strengthen the recrystallization of absorption precursor and can promote merging process between island and the island, improve the crystalline quality of epitaxial film.But too high growth temperature can make speed of response become too fast, generates ZnTe so that precursor has little time to adjust the position with regard to immediate response, forms easily the room and sneaks into impurity, thereby crystalline quality is descended.Simultaneously, the diffusion of contaminants that high growth temperature can increase in the substrate enters epitaxial film, thereby reduces the quality of epitaxial film.Preferred growth temperature is 400 ° of C.
The ZnTe homogeneity epitaxial layer of the inventive method preparation has narrow band edge exciton peak and narrow XRC halfwidth, and oxygen bound exciton and the deep level emissions such as Y line relevant with dislocation do not occur, and these results show that epitaxial film has good crystalline quality.
The ZnTe homogeneity epitaxial layer of the inventive method preparation can be used for the preparation of green light LED and the photoelectric devices such as LD and terahertz transmitter, is with a wide range of applications.
Description of drawings
Fig. 1 is the low temperature PL spectrum of the ZnTe homogeneity epitaxial layer of the differential responses chamber pressure (300,500 and 700Torr) with the inventive method preparation.Exciting power is 2mW, and excitation wavelength 442nm, LASER SPECKLE diameter are 250 μ m, and the measurement temperature is 6K.Wherein, X-coordinate: photon energy/eV; Ordinate zou: luminous intensity/arbitrary unit.The PL spectrum of all epitaxial films all shows to have narrow band edge exciton peak (free exciton FE (1s), neutral donor bound exciton I
dOr neutral acceptor bound exciton I
a), deep level emission and the Y line relevant with dislocation do not appear.Along with the increase of chamber pressure, the glow peak relevant with impurity (bound exciton and alms giver acceptor to) strengthens gradually, illustrates that the ZnTe epitaxial film of growing under the low pressure has better optical quality.
Fig. 2 is the ZnTe epitaxial film X-ray diffraction spectrum (XRD) of growing under the 300Torr of the inventive method preparation.Wherein, X-coordinate: 2 θ/degree; Ordinate zou: intensity/arbitrary unit.Only observe ZnTe(200 among the XRD) and the diffraction peak of (400) face, reflected to illustrate the iso-epitaxy relation of substrate and epitaxial film not have stress relief in the epitaxial film.
Fig. 3 is the X ray rocking curve (XRC) of (400) face of ZnTe homogeneity epitaxial layer of the differential responses chamber pressure (300,500 and 700Torr) of the inventive method preparation.Wherein, X-coordinate: Δ ω/rad; Ordinate zou: intensity/arbitrary unit.Along with chamber pressure increases, the halfwidth of ZnTe epitaxial film XRC obviously increases, and illustrates that the ZnTe epitaxial film of growing under the low pressure has better crystalline quality.
Embodiment
The present invention will be further described below by embodiment, but be not limited to this.
Embodiment 1:
A kind of preparation method of zinc telluridse homogeneity epitaxial layer, adopt metal organic chemical vapor deposition technique, take zinc methide and tellurium diethyl as metal organic source, with hydrogen as carrier gas, with low pressure metal organic chemistry vapour phase epitaxy equipment at ZnTe(100) Grown zinc telluridse epitaxial film; Its processing condition are as follows:
Underlayer temperature during growth: 400 ° of C;
Chamber pressure: 300Torr;
Zinc methide transports speed: 15 μ mol/min;
Tellurium diethyl transports speed: 15 μ mol/min;
Growth time: 3 hours
Above-mentioned preparation method's operation steps is as follows:
1, the cleaning of ZnTe substrate: with the ultrasonic cleaning after 5 minutes in organic solvent-acetone of (100) face ZnTe substrate, be put in the 1% bromine methanol solution immersion treatment 30 minutes, rinse well with deionized water at last;
2, the MOVPE equipment reaction chamber is passed into H
2, kept 30 minutes at 470 ° of C, remove the oxide compound of ZnTe substrate surface;
3, underlayer temperature is controlled at 400 ° of C, regulates hydrogen flowing quantity, make zinc methide (DMZn) and tellurium diethyl (DETe) transport speed and all maintain 15 μ mol/min, control chamber pressure at 300Torr, growth time 3 hours;
4, growth finishes, and closes zinc source and tellurium source, and the stopped heating substrate is at ZnTe(100) Grown goes out the ZnTe epitaxial film, continues to pass into hydrogen 30 minutes, is down to room temperature.
Compare with the epitaxial film of growing under other underlayer temperatures and the chamber pressure, the zinc telluridse epitaxial film of growing under 400 ° of C of underlayer temperature and the chamber pressure 300Torr, its low temperature PL composes demonstration, FREE EXCITON EMISSION IN FORWARD peak (FE (1s)) is dominant, halfwidth is very little, be about 3meV, can be observed the clearly excited state of free exciton (FE (2s)) and LO phonon replica (FE (1s)-LO), the alms giver acceptor does not appear to emission band (DAP), do not observe simultaneously Y line and other deep level emissions, show that the ZnTe epitaxial film of this condition growth has good optical quality (seeing accompanying drawing 1).The X ray rocking curve (XRC) of (400) face of epitaxial film shows that along with chamber pressure increases, the halfwidth of ZnTe epitaxial film XRC obviously increases, and illustrates that the ZnTe epitaxial film of growing under the 300Torr has best crystalline quality (seeing accompanying drawing 3).
Embodiment 2:
Processing condition are as follows:
Chamber pressure: 700Torr;
Underlayer temperature during growth: 380 ° of C;
Zinc methide transports speed: 10 μ mol/min;
Tellurium diethyl transports speed: 10 μ mol/min;
Growth time: 4 hours.
Low pressure MOVPE technique prepares the zinc telluridse epitaxial film, and step is as follows:
1, the cleaning of ZnTe substrate: with the ultrasonic cleaning after 5 minutes in organic solvent-acetone of (100) face ZnTe substrate, be put in the 1% bromine methanol solution immersion treatment 20 minutes, rinse well with deionized water at last;
2, the MOVPE equipment reaction chamber is passed into H
2, kept 30 minutes at 550 ° of C, remove the oxide compound of ZnTe substrate surface;
3, underlayer temperature is controlled at 380 ° of C, regulates hydrogen flowing quantity, make zinc methide (DMZn) and tellurium diethyl (DETe) transport speed and all maintain 10 μ mol/min, control chamber pressure at 700Torr, growth time 4 hours;
4, growth finishes, and closes zinc source and tellurium source, and the stopped heating substrate is at ZnTe(100) Grown goes out the ZnTe epitaxial film, continues to pass into hydrogen 30 minutes, is down to room temperature.
Embodiment 3:
Processing condition are as follows:
Underlayer temperature during growth: 420 ° of C;
Chamber pressure: 500Torr;
Zinc methide transports speed: 30 μ mol/min;
Tellurium diethyl transports speed: 30 μ mol/min;
Growth time: 2 hours;
MOVPE technique prepares the zinc telluridse epitaxial film, and step is as follows:
1, the cleaning of ZnTe substrate: with the ultrasonic cleaning after 5 minutes in organic solvent-acetone of (100) face ZnTe substrate, be put in the 1% bromine methanol solution immersion treatment 20 minutes, rinse well with deionized water at last;
2, the MOVPE equipment reaction chamber is passed into H
2, kept 30 minutes at 420 ° of C, remove the oxide compound of ZnTe substrate surface;
3, underlayer temperature is controlled at 420 ° of C, regulates hydrogen flowing quantity, make zinc methide (DMZn) and tellurium diethyl (DETe) transport speed and all maintain 30 μ mol/min, control chamber pressure at 500Torr, growth time 2 hours;
4, growth finishes, and closes zinc source and tellurium source, and the stopped heating substrate is at ZnTe(100) Grown goes out the ZnTe epitaxial film, continues to pass into hydrogen 30 minutes, is down to room temperature.
Embodiment 4:(Comparative Examples)
MOVPE technique prepares the zinc telluridse epitaxial film, and preparation technology is identical with embodiment 1, just:
Underlayer temperature during growth: 440 ° of C;
Growth time: 2 hours, identical among the epitaxy layer thickness of preparation and the embodiment 1;
Compare the crystalline quality variation of the zinc telluridse epitaxial film of growing under these processing condition with embodiment 1.This is because the diffusion of contaminants that high growth temperature forms in room and the increase substrate easily enters epitaxial film, thereby crystalline quality is descended.
Embodiment 5:(Comparative Examples)
MOVPE technique prepares the zinc telluridse epitaxial film, and preparation technology is identical with embodiment 1, just growth conditions:
Chamber pressure: 700Torr;
Growth time: 2 hours, the epitaxy layer thickness of preparation was identical with embodiment 4 with embodiment 1;
The PL spectrum of the zinc telluridse epitaxial film of growing under these processing condition shows the glow peak relevant with impurity (DAP, I
aAnd I
dDeng) dominant (accompanying drawing 1), simultaneously, the XRC test shows that the rising chamber pressure can increase the halfwidth of the XRC of ZnTe epitaxial film, and the crystalline quality variation (accompanying drawing 3) of the ZnTe epitaxial film of this condition growth is described.
Embodiment 6:(Comparative Examples)
MOVPE technique prepares the zinc telluridse epitaxial film, and preparation technology is identical with embodiment 1, just growth conditions:
Chamber pressure: 100Torr;
Growth time: 5 hours,
Under this chamber pressure, restive very desirable of experiment condition, difficulty is accurately implemented in experiment, and simultaneously, chamber pressure is less, and the speed of outer layer growth is less, can increase production cost, so the Optimal Growing air pressure of the inventive method is 300Torr.
Claims (4)
1. the preparation method of a zinc telluridse homogeneity epitaxial layer, adopt low pressure metal organic chemistry process for vapor phase epitaxy, take zinc methide and tellurium diethyl as metal organic source, as carrier gas, use low pressure metal organic chemistry vapour phase epitaxy equipment at ZnTe(100 with hydrogen) Grown zinc telluridse epitaxial film; Its processing condition are as follows:
Chamber pressure: 100-760Torr;
Underlayer temperature during growth: 380-460 ° C;
Zinc methide transports speed: 10-30 μ mol/min;
Tellurium diethyl transports speed: 10-30 μ mol/min;
Growth time: 2-10 hour.
2. the preparation method of a kind of zinc telluridse homogeneity epitaxial layer as claimed in claim 1 is characterized in that its operation steps is as follows:
1) cleaning of ZnTe substrate: (100) face ZnTe substrate in organic solvent-acetone after ultrasonic cleaning 3-5 minute, is put in the 1% bromine methanol solution at immersion treatment 20-30 minute, rinses well with deionized water at last;
2) the MOVPE equipment reaction chamber is passed into H
2, kept 20-40 minute at 500-600 ° of C, remove the oxide compound of ZnTe substrate surface;
3) underlayer temperature is controlled at 380-460 ° of C, regulate hydrogen flowing quantity, make zinc methide (DMZn) and tellurium diethyl (DETe) transport speed and all maintain 10-30 μ mol/min, control chamber pressure at 100-760Torr, growth time 2-10 hour;
4) growth finishes, and closes zinc source and tellurium source, and the stopped heating substrate is at ZnTe(100) Grown goes out the ZnTe epitaxial film, continues to pass into hydrogen 20-30 minute, is down to room temperature.
3. the preparation method of a kind of zinc telluridse homogeneity epitaxial layer as claimed in claim 1 is characterized in that its processing condition are as follows:
Underlayer temperature during growth: 400 ° of C;
Chamber pressure: 300Torr;
Zinc methide transports speed: 15 μ mol/min;
Tellurium diethyl transports speed: 15 μ mol/min;
Growth time: 3 hours.
4. the preparation method of a kind of zinc telluridse homogeneity epitaxial layer as claimed in claim 1 is characterized in that described zinc methide purity is 99.9999%; Tellurium diethyl purity is 99.9999%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103474333A (en) * | 2013-09-16 | 2013-12-25 | 中国科学院半导体研究所 | Doping method for p-type zinc telluride single crystal thin-film material |
| CN104746143A (en) * | 2015-03-05 | 2015-07-01 | 中国电子科技集团公司第十一研究所 | Molecular beam epitaxy process method for silicon-based zinc telluride buffer layer |
| CN106992792A (en) * | 2017-05-23 | 2017-07-28 | 中国电子科技集团公司第十三研究所 | 220GHz terahertz sources machines based on MEMS technology |
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| CN103474333A (en) * | 2013-09-16 | 2013-12-25 | 中国科学院半导体研究所 | Doping method for p-type zinc telluride single crystal thin-film material |
| CN104746143A (en) * | 2015-03-05 | 2015-07-01 | 中国电子科技集团公司第十一研究所 | Molecular beam epitaxy process method for silicon-based zinc telluride buffer layer |
| CN106992792A (en) * | 2017-05-23 | 2017-07-28 | 中国电子科技集团公司第十三研究所 | 220GHz terahertz sources machines based on MEMS technology |
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