CN104357798A - CdZnOS quaternary ZnO alloy semiconductor material and preparation method thereof - Google Patents

CdZnOS quaternary ZnO alloy semiconductor material and preparation method thereof Download PDF

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CN104357798A
CN104357798A CN201410571284.XA CN201410571284A CN104357798A CN 104357798 A CN104357798 A CN 104357798A CN 201410571284 A CN201410571284 A CN 201410571284A CN 104357798 A CN104357798 A CN 104357798A
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cdznos
semiconductor material
alloy semiconductor
powder
quaternary
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CN104357798B (en
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何云斌
黎明锴
郑丽兰
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Hubei University
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/28—Vacuum evaporation by wave energy or particle radiation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth

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Abstract

The invention discloses a CdZnOS quaternary ZnO alloy semiconductor material and a preparation method thereof. The preparation method comprises the following steps: enabling Cd and S to be simultaneously doped with ZnO, and adjusting the ratio of Cd to Zn to O to S in CdZnOS to form the brand-new CdZnOS quaternary ZnO alloy semiconductor material, wherein a wide bandgap semiconductor with a bandgap adjustable within a relatively wide range is obtained and can be used for luminescent devices or light detection devices. A reported CdZnOS single-crystal material is successfully synthesized for the first time in the world, and the preparation of the CdZnOS quaternary ZnO alloy semiconductor is of great significance on development of wavelength-adjustable photoelectric devices; the CdZnOS quaternary ZnO alloy semiconductor material can grow by various methods of conventional pulsed laser deposition, magnetron sputtering, electron beam evaporation and the like; equipment and the operation process are simple, and the control is easy.

Description

A kind of CdZnOS quaternary ZnO alloy semiconductor material and preparation method thereof
Technical field
The invention belongs to photoelectric semiconductor material preparation field, particularly a kind of CdZnOS quaternary ZnO alloy semiconductor material and preparation method thereof.
Background technology
Third generation wide bandgap semiconductor ZnO has the energy gap of about 3.3eV, the exciton bind energy of 60 meV, has purposes widely in photoelectric device.Adulterate to realize its band-gap tuning to ZnO, the wavelength region that it uses can be widened, realize device application widely.As in zno-based semiconductor material, replace Zn with Cd, obtain by the CdZnO of certain component solid solution, there is the forbidden band narrower compared with ZnO by ZnO and CdO.Experiment proves, can realize CdZnO band gap by the dull continuously adjustabe of 3.3eV to 1.8eV by the content changing Cd.On the other hand, except replacing Zn with positively charged ion 2+, the O of ZnO can also be replaced by negatively charged ion 2-realize the band-gap tuning of ZnO.As replaced the O in ZnO with S, obtain can be with to ZnO the ZnOS material regulated.Research shows, a small amount of S doped and substituted O can raise the valence band of ZnO, forms the top of valence band of class ZnS, can effectively reduce the band gap of ZnO.When S content about 50%, the minimum about 2.6eV of band gap of ZnOS.These doping all effectively can realize continuously adjustable low band gaps zno-based semiconductor material, have widened the gesture hydrazine layer material of zno-based semiconductor material as quantum well devices or the wavelength region of photoelectric device active layer.Cd and S co-doped ZnO can realize its low band gaps continuously adjustabe, and the novel C dZnOS quaternary semiconductor material under the doping of high Cd content and appropriate S, comparatively CdZnO and ZnOS sill is lower to be expected to make band gap, and this photoelectric device for exploitation visible light wave range is significant.
At present some report about CdZnO and ZnOS semiconductor material, but there is not yet Cd and S mixes the report that ZnO prepares CdZnOS quaternary ZnO alloy semiconductor material jointly.The present invention prepares CdZnOS quaternary ZnO alloy semiconductor material first, has very important significance for photoelectric device such as research and development visible light wave range luminescent device or photo-detector etc.
Summary of the invention
For the multiple degree of freedom realized ZnO can be with regulates, we have invented a kind of preparation method of CdZnOS quaternary ZnO alloy semiconductor material, the preparation method of described CdZnOS quaternary ZnO alloy semiconductor material comprises the following steps:
Step 1, the stupalith needed for preparation growth CdZnOS quaternary ZnO alloy semiconductor film material.
Take high-purity ZnS and CdO powder according to a certain ratio, the molar ratio of described ZnS powder and CdO powder is 95:5 ~ 60:40;
The deionized water adding powder total mass 60% in the above-mentioned powder taken carries out ball milling;
Powder after ball milling is carried out vacuum drying treatment, and in loft drier, vacuum tightness is 0.1Pa, and temperature is 100 DEG C, dry 6 hours;
Add the deionized water of powder quality 6% in above-mentioned mixed powder after the drying, grinding stirring makes powder Homogeneous phase mixing be bonded together;
Homomixture is placed in mould, is pressed into ceramic green sheet, the thickness of ceramic green sheet is 2mm;
Ceramic green sheet is put into vacuum tube furnace, and around ceramic green sheet, places sulphur powder, under argon shield, obtain required ceramic target at 600 ~ 700 DEG C of high temperature sinterings after 3 ~ 4 hours.
Step 2, adopts pulse laser ablation method to prepare CdZnOS film.
Adopt the stupalith of step 1 preparation as laser ablation target, adopt sapphire as the substrate of film growth;
By one or more reagent ultrasonic cleaning in acetone, dehydrated alcohol and deionized water of substrate 15 minutes;
The substrate that target step 1 prepared and above-mentioned cleaning obtain is placed on respectively in target platform and sample table and loads vacuum chamber, and opens vacuum pump evacuation, and vacuum tightness is 10 -4below Pa, the growth temperature regulating substrate is 700 DEG C, opens sample table and the rotation of target platform;
Pass into oxygen, adjustment oxygen pressure is 0.05 ~ 2.5Pa, opens laser apparatus, and ceramic target surface atom laser ablation is out deposited on substrate surface and forms CdZnOS film, laser energy is 250 ~ 300mJ/pulse.
By CdZnOS quaternary ZnO alloy semiconductor material will be obtained in Cd and S co-doped to ZnO.
Described CdZnOS quaternary ZnO alloy semiconductor material is thin-film material.
By the content regulating the oxygen pressure in target Raw proportioning and thin film growth process to regulate Cd, S in CdZnOS quaternary ZnO alloy semiconductor material, to realize the adjustment to ZnO band gap, thus the operation wavelength of regulation and control photoelectric device.
Beneficial effect of the present invention is:
1, the CdZnOS quaternary ZnO alloy semiconductor material obtained by Cd, S co-doped ZnO, the doping content by adjustment Cd, S realizes the adjustment to ZnO band gap, thus the operation wavelength controlling photoelectric device moves to visible light wave range.Preparation CdZnOS quaternary ZnO alloy semiconductor material has very important significance for the photoelectric device of exploitation visible-range Wavelength tunable.
2, CdZnOS quaternary ZnO alloy semiconductor material of the present invention can adopt the multiple semiconductor material growing methods such as conventional pulsed laser deposition, magnetron sputtering, electron beam evaporation to grow, and equipment and operating procedure simply, are easy to control.
Accompanying drawing explanation
Fig. 1 is that the X-ray diffraction (XRD) of CdZnOS film prepared by the present invention tests collection of illustrative plates;
Fig. 2 is x-ray photoelectron power spectrum (XPS) figure of CdZnOS film prepared by the present invention;
Fig. 3 is the transmitted light spectrogram that the present invention grows the CdZnOS film of preparation under different oxygen press strip part.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is described in further detail, but example is not as a limitation of the invention.
Embodiment 1
Take ZnS powder 21.8880 grams and CdO powder 8.1120 grams (mol ratio ZnS:CdO=80:20) and be placed in ball grinder, add deionized water 18mL ball milling 4 hours, afterwards at 100 DEG C, under 0.1Pa in vacuum drying oven dry 6 hours.Dried powder is added 1.8mL deionized water and fully grind the circular blank that the rear compressing tablet of stirring becomes diameter 21mm, thickness 2mm.Blank is put into crucible and is placed on vacuum tube furnace, and around it, put the identical powder of composition and high purity sulphur powder.High-purity argon gas is passed into after vacuum tube furnace being evacuated to 0.1Pa.Under protective atmosphere, tube furnace be warming up to 600 DEG C and be incubated 3 hours, naturally cooling to room temperature subsequently, obtaining required stupalith.Using this stupalith as laser ablation target, c surface sapphire is as substrate.By substrate successively through acetone, dehydrated alcohol and deionized water etc. respectively ultrasonic cleaning load vacuum chamber after 15 minutes together with target, and be evacuated to 10 -4pa.Open silicon and regulate underlayer temperature to be 700 DEG C.Pass into oxygen, make air pressure maintain 2.0Pa in whole film deposition process.Opening sample table rotating speed is 10r/min, target platform rotation 5r/min.Setting laser device is permanent energy pattern, and output energy is 250mJ/pulse, and pulse-repetition frequency is 5Hz, pulse number 9000.Open laser splash and close silicon after 30 minutes.Sample takes out vacuum chamber after naturally cooling to room temperature in a vacuum.
The CdZnOS quaternary ZnO alloy semiconductor film material prepared for the present embodiment carries out XRD and the test of x-ray photoelectron power spectrum, and test result as depicted in figs. 1 and 2.As can be seen from Figure 1, only there is the diffraction peak of (002) and (004) of CdZnOS film in the XRD figure spectrum of this material, prove the CdZnOS film of the high C-axis preferred orientation obtaining pure wurtzite phase; The characteristic peak of Cd, Zn, O and S tetra-kinds of elements has been there is, containing these four kinds of elements in the film prepared by proving in x-ray photoelectron energy spectrogram.
Embodiment 2
Take ZnS powder 21.8880 grams and CdO powder 8.1120 grams (mol ratio ZnS:CdO=80:20) and be placed in ball grinder, add deionized water 18mL ball milling 4 hours, afterwards at 100 DEG C, under 0.1Pa in vacuum drying oven dry 6 hours.Dried powder adds 1.8mL deionized water and fully grinds the circular blank that the rear compressing tablet of stirring becomes diameter 21mm, thickness 3mm.Blank is put into crucible and is placed on vacuum tube furnace, and around it, put the identical powder of composition and sulphur powder.High-purity argon gas is passed into after vacuum tube furnace being evacuated to 0.1Pa.Under protective atmosphere, tube furnace be warming up to 600 DEG C and be incubated 3 hours, naturally cooling to room temperature subsequently, obtaining required stupalith.Using this stupalith as laser ablation target, using c surface sapphire as substrate.By substrate successively through acetone, dehydrated alcohol and deionized water etc. respectively ultrasonic cleaning load vacuum chamber after 15 minutes together with target, and be evacuated to 10 -4pa.Open silicon and regulate underlayer temperature to be 700 DEG C.Pass into oxygen, make air pressure remain constant in whole film deposition process: oxygen press strip part is respectively 0.05Pa, 1.0Pa and 2.0Pa, to prepare the CdZnOS thin-film material of different S content.Opening sample table rotating speed is 10r/min, target platform rotation 5r/min.Setting laser device is permanent energy pattern, and output energy is 250mJ/pulse, and pulse-repetition frequency is 5Hz, pulse number 9000.Open laser splash and close oxygen and silicon after 30 minutes.Sample takes out vacuum chamber after naturally cooling to room temperature in a vacuum.
The CdZnOS quaternary ZnO alloy semiconductor film material prepared under different oxygen press strip part (0.05Pa, 1.0Pa and 2.0Pa) to the present embodiment carries out transmitted spectrum test, and result as shown in Figure 3.As seen from the figure, along with the rising of oxygen pressure, the ABSORPTION EDGE of CdZnOS film, towards the red shift of long-wave band direction, illustrates that its energy bandgaps reduces gradually, enters visible light wave range.Therefore, CdZnOS thin-film material can be used as the active layer of visible light wave range photoelectric device.
Embodiment 3
Take ZnS powder 13.9143 grams and CdO powder 1.0857 grams (mol ratio ZnS:CdO=95:5) and be placed in ball grinder, add deionized water 9mL ball milling 4 hours, afterwards at 100 DEG C, under 0.1Pa in vacuum drying oven dry 6 hours.Dried powder adds 0.9mL deionized water and fully grinds the circular blank that the rear compressing tablet of stirring becomes diameter 21mm, thickness 2mm.Blank is put into crucible and is placed on vacuum tube furnace, and around it, put the identical powder of composition and high purity sulphur powder.High-purity argon gas is passed into after vacuum tube furnace being evacuated to 0.1Pa.Under protective atmosphere, tube furnace be warming up to 700 DEG C and be incubated 3 hours, naturally cooling to room temperature subsequently, obtaining required stupalith.Using this stupalith as laser ablation target, using c surface sapphire as substrate.By substrate successively through acetone, dehydrated alcohol and deionized water etc. respectively ultrasonic cleaning load vacuum chamber after 15 minutes together with target, and be evacuated to 10 -4pa.Open silicon and regulate underlayer temperature to be 700 DEG C.Pass into oxygen, make air pressure maintain 2.3Pa in whole film deposition process.Opening sample table rotating speed is 10r/min, target platform rotation 5r/min.Setting laser device is permanent energy pattern, and output energy is 300mJ/pulse, and pulse-repetition frequency is 5Hz, pulse number 18000.Open laser deposition and close oxygen and silicon after 60 minutes.Sample takes out vacuum chamber after naturally cooling to room temperature in a vacuum.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (4)

1. CdZnOS quaternary ZnO alloy semiconductor material and preparation method thereof, is characterized in that, the preparation method of described CdZnOS quaternary ZnO alloy semiconductor material comprises the following steps:
Step 1, the ceramic target needed for preparation growth CdZnOS quaternary ZnO alloy semiconductor film material,
1.1, take high-purity ZnS and CdO powder according to a certain ratio, the molar ratio of described ZnS powder and CdO powder is 95:5 ~ 60:40;
1.2, the deionized water adding powder total mass 60% in the above-mentioned powder taken carries out ball milling;
1.3, the powder after ball milling is carried out vacuum drying treatment, in loft drier, vacuum tightness is 0.1Pa, and temperature is 100 DEG C, dry 6 hours;
1.4, add the deionized water of powder quality 6% in above-mentioned mixed powder after the drying, grinding stirring makes powder Homogeneous phase mixing be bonded together;
1.5, homomixture is placed in mould, is pressed into ceramic green sheet, the thickness of ceramic green sheet is 2mm;
1.6, ceramic green sheet is put into vacuum tube furnace, and around ceramic green sheet, place sulphur powder, under argon shield, obtain required stupalith at 600 ~ 700 DEG C of high temperature sinterings after 3 ~ 4 hours;
Step 2, adopts pulse laser ablation method to prepare CdZnOS film,
2.1, the stupalith adopting step 1 to prepare, as laser ablation target, adopts sapphire as the substrate of film growth;
2.2, by one or more reagent ultrasonic cleaning in acetone, dehydrated alcohol and deionized water of substrate 15 minutes;
2.3, target step 1 prepared and step 2.2 are cleaned the substrate obtained and are placed on respectively in target platform and sample table and load vacuum chamber, and open vacuum pump evacuation, and vacuum tightness is 10 -4below Pa, the growth temperature regulating substrate is 700 DEG C, opens sample table and the rotation of target platform;
2.4, pass into oxygen, adjustment oxygen pressure is 0.05 ~ 2.5Pa, opens laser apparatus, and ceramic target surface atom laser ablation is out deposited on substrate surface and forms CdZnOS film, laser energy is 250 ~ 300mJ/pulse.
2. the CdZnOS quaternary ZnO alloy semiconductor material that obtains of preparation method according to claim 1, is characterized in that, by obtaining CdZnOS quaternary ZnO alloy semiconductor material in Cd and S co-doped to ZnO.
3. CdZnOS quaternary ZnO alloy semiconductor material according to claim 2, is characterized in that, described CdZnOS quaternary ZnO alloy semiconductor material is thin-film material.
4. CdZnOS quaternary ZnO alloy semiconductor material according to claim 2, it is characterized in that, by the content regulating the oxygen pressure in target Raw proportioning and thin film growth process to regulate Cd, S in CdZnOS quaternary ZnO alloy semiconductor material, to realize the adjustment to ZnO band gap, thus the operation wavelength of regulation and control photoelectric device.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105332048A (en) * 2015-10-20 2016-02-17 江苏大学 Zinc oxide-based alloy semi-conducting material, and preparation method thereof
CN105800671A (en) * 2016-03-08 2016-07-27 湖北大学 BeCdZnO compound semiconductor material with tunable band gap and preparation method of BeCdZnO compound semiconductor material

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101506959A (en) * 2006-06-22 2009-08-12 株式会社藤仓 Method for producing zinc oxide semiconductor crystal
CN102851644A (en) * 2012-09-07 2013-01-02 昆山铭佳利电子制品有限公司 Preparation method for photoelectric material
CN103074576A (en) * 2013-02-04 2013-05-01 清华大学 ZnO-based diluted magnetic semiconductor thin film and preparation method thereof
JP5506221B2 (en) * 2009-03-26 2014-05-28 スタンレー電気株式会社 Method for manufacturing ZnO-based semiconductor element
CN103952669A (en) * 2014-04-23 2014-07-30 北京工业大学 Method for regulating and controlling visible light emitting type of intrinsic zinc oxide film

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101506959A (en) * 2006-06-22 2009-08-12 株式会社藤仓 Method for producing zinc oxide semiconductor crystal
JP5506221B2 (en) * 2009-03-26 2014-05-28 スタンレー電気株式会社 Method for manufacturing ZnO-based semiconductor element
CN102851644A (en) * 2012-09-07 2013-01-02 昆山铭佳利电子制品有限公司 Preparation method for photoelectric material
CN103074576A (en) * 2013-02-04 2013-05-01 清华大学 ZnO-based diluted magnetic semiconductor thin film and preparation method thereof
CN103952669A (en) * 2014-04-23 2014-07-30 北京工业大学 Method for regulating and controlling visible light emitting type of intrinsic zinc oxide film

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105332048A (en) * 2015-10-20 2016-02-17 江苏大学 Zinc oxide-based alloy semi-conducting material, and preparation method thereof
CN105800671A (en) * 2016-03-08 2016-07-27 湖北大学 BeCdZnO compound semiconductor material with tunable band gap and preparation method of BeCdZnO compound semiconductor material

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