CN105734491A - BeZnOS compound semiconductor material as well as preparation method and application thereof - Google Patents
BeZnOS compound semiconductor material as well as preparation method and application thereof Download PDFInfo
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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
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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Abstract
The invention belongs to the technical field of a semiconductor photoelectric material, and particularly relates to a BeZnOS compound semiconductor material as well as a preparation method and application thereof. The BeZnOS material provided by the invention is a quaternary compound semiconductor material which is obtained by solid solution treatment of BeO and ZnS in a certain proportion; and through the synergistic effect of compound substituting of Be and S, not only the relatively free regulation of ZnO band gaps can be realized, but also the effects of improving the solubility of substituting elements, namely Be and S in ZnO and eliminating the mutual dependence between solid solution band gaps and lattice constant regulation are also achieved. The BeZnOS quaternary compound is a wide band gap semiconductor with free adjustable band gaps and can be applied to an ultraviolet solstice dead zone luminescent device or an optical detector. The BeZnOS compound semiconductor material provided by the invention can grow by adopting multiple methods such as pulsed laser deposition, magnetron sputtering and electron beam evaporation, and equipment and operation technologies are simple. The BeZnOS single crystal thin-film material provided by the invention is successfully synthesized for the first time in the world and has very important significance for development of ZnO-based photoelectric devices with adjustable wavelength.
Description
Technical field
The invention belongs to photoelectric semiconductor material technical field, be specifically related to a kind of BeZnOS compound semiconductor materials, its preparation method and application.
Background technology
Third generation wide bandgap semiconductor ZnO has the exciton bind energy of the energy gap of 3.3eV, 60meV, has potential extensive use in blue light, UV-light luminous and photodetection etc..For realizing device application, generally require and ZnO is carried out substitute doping, can be with regulating it.Broader forbidden band can be obtained as obtained BeZnO ternary compound with Be part replacement Zn.BeZnO is formed by certain component ratio solid solution by ZnO and BeO, BeO and ZnO is all hexagonal structure, BeO energy gap (10.8eV) is far longer than ZnO, therefore a small amount of Be of solid solution in ZnO is had only to, it is possible to while expanding energy gap, the hexagonal wurtzite structure of ZnO can be kept again.Can realizing the dull continuously adjustabe to BeZnO band gap by changing the content of Be, therefore BeZnO can as the active layer of the abarrier layer material of zno-based quantum well devices or ultraviolet light detector.Except Zn can be replaced by cation2+, moreover it is possible to replace O by anion2-Regulate the band gap of ZnO.As replaced the O in ZnO with S portion, obtain ZnOS, it is possible to realize the ZnO adjustment that can be with.Replacing Zn from Be different, a small amount of S replaces O can raise the valence band of ZnO, forms the top of valence band of class ZnS, reduces band gap.When S content about 50%, the minimum about 2.6eV of band gap of ZnOS.When the content of S increases further, the band gap of ZnOS also can increase therewith.The covalent radius difference of Be and Zn is very big, and (Zn isIt is significantly greater than Be's), Be doping zinc-oxide is excessive due to differences between lattice constant, can cause the limited solubility of thin film crystallization degradation and Be, and therefore we are simultaneously introduced the S that covalent radius is biggerPartly replace O (covalent radius), to reach the complementary effect with increase substituted element dissolubility of lattice paprmeter.The BeZnOS quaternary solid solution compound semi-conducting material of this invention design, regulate solid solution band gap with Be element for main and regulate solid solution lattice constant with S element for main, so while reaching freely to regulate and control BeZnOS quaternary compound band gap purpose, it is possible to resolve in ternary BeZnO, ZnOS solid solution, substituted element dissolubility finite sum solid solution band gap regulates, with lattice paprmeter, the problem mutually pind down.At present about some report of BeZnO and ZnOS semi-conducting material, but there is not yet the report preparing BeZnOS quaternary compound semiconductor material.
Summary of the invention
For solving the deficiencies in the prior art, the invention provides a kind of BeZnOS compound semiconductor materials, its preparation method and application.
A kind of BeZnOS compound semiconductor materials, the quaternary compound semiconductor material obtained for BeO and ZnS solid solution.
The preparation method that present invention also offers a kind of BeZnOS quaternary compound semiconductor material, comprises the following steps:
1) ceramic target needed for BeZnOS compound semiconductor film material is prepared, described ceramic target is obtained by ceramic green sheet sintering, wherein, described ceramic green sheet includes ZnS and the BeO that mol ratio is 99:1～70:30, the sintering temperature of described ceramic green sheet is 700～1250 DEG C, and sintering time is 4～6 hours.
Step 1) comprise the following steps:
1.1) weigh ZnS powder and BeO powder that mol ratio is 99:1～70:30, obtain just mixed powder；
1.2) to step 1.1) deionized water that adds just mixed powder gross mass 50～70% in the first mixed powder that obtains carries out ball milling, obtains mixed-powder；
1.3) by step 1.2) mixed-powder that obtains carries out vacuum drying treatment, obtains the mixed-powder dried, and wherein, background pressure≤0.1Pa, baking temperature is 100～120 DEG C, and drying time is 6～8 hours；
1.4) to step 1.3) the dry mixed-powder that obtains adds the dehydrated alcohol of dry mixed-powder gross mass 2～6%, grinding stirs, and obtains mixing the ceramic batch being bonded together；
1.5) by step 1.4) ceramic batch that obtains is pressed into ceramic green sheet；
1.6) with sulfur powder for oxygen scavenger, with argon for protection gas, to step 1.5 in vacuum tube furnace) ceramic green sheet that obtains is sintered, and obtains ceramic target.
2) with sapphire for substrate, pulsed laser ablation deposition method is adopted to carry out the growth of BeZnOS thin film over the substrate described ceramic target, obtain BeZnOS quaternary compound semiconductor material, wherein, underlayer temperature is 25～1000 DEG C, laser energy is 250～600mJ/pulse, and oxygen pressure is 0～10Pa.
Step 2) comprise the following steps:
2.1) substrate grown as thin film using sapphire, and substrate is carried out ultrasonic waves for cleaning and dry, obtain clean substrate, wherein, cleanout fluid is any one or a few the mixing in acetone, dehydrated alcohol and deionized water, and scavenging period is 10～20 minutes；
2.2) under the atmospheric condition of oxygen, to step 1) ceramic target that obtains adopts pulsed laser ablation deposition method in step 2.1) the clean substrate that obtains carries out the growth of BeZnOS thin film.
Said method provided by the present invention is by obtaining BeZnOS quaternary compound semiconductor material by BeO and ZnS solid solution.
Present invention also offers the BeZnOS quaternary compound semiconductor material that the preparation method according to above-mentioned BeZnOS compound semiconductor materials prepares.
BeZnOS compound semiconductor materials provided by the present invention can also carry out growth preparation by the multiple method such as magnetron sputtering, electron beam evaporation.
BeZnOS compound semiconductor materials provided by the present invention can be thin-film material.
Present invention also offers the application of above-mentioned BeZnOS compound semiconductor materials, as the active layer of the abarrier layer material of zno-based quantum well devices or blue light, ultraviolet light detector.
Above-mentioned material provided by the present invention realizes the adjustment to ZnO band gap by regulating the content of Be, S, thus controlling the operation wavelength of photoelectric device, moreover it is possible to by regulating valence band and the conduction band structure of ZnO, change its electronics and hole characteristic.
The invention have the benefit that
1, pass through that Be, S are solid-solution in ZnO jointly and obtain BeZnOS quaternary compound semiconductor material, the adjustment to ZnO band gap can not only be realized by the content of adjustment Be, S, thus controlling the operation wavelength of photoelectric device, valence band and the conduction band structure of ZnO can also be regulated, reduce at the bottom of conduction band, adjust each energy level relatively preparing in relation and conduction band of each point of band in conduction band, improve top of valence band, adjust each energy level relatively preparing in relation and valence band of each point of band in valence band, improve its electronics and hole characteristic.The synergism that Be, S compound replaces, not only can realize the freer regulation and control to ZnO band gap, also acts as and increases substituted element Be, S dissolubility in solid solution and eliminate the effect that solid solution band gap pins down mutually with lattice paprmeter adjustment.The BeZnOS quaternary compound semiconductor material of design preparation has very important significance for the photoelectric device developing Wavelength tunable.
2, the BeZnOS quaternary compound semiconductor material of the present invention can adopt the multiple methods such as conventional pulsed laser ablation deposition, magnetron sputtering, electron beam evaporation to grow, and equipment and operating procedure are simple, it is easy to controls.
3, the BeZnOS quaternary compound semiconductor thin-film material of the present invention has good degree of crystallinity, obtains its crystallite dimension by x-ray diffraction test and is about 35nm.
Accompanying drawing explanation
The X-ray diffraction (XRD) that Fig. 1 is BeZnOS thin film prepared by the present invention tests collection of illustrative plates；
Fig. 2 is x-ray photoelectron power spectrum (XPS) figure of BeZnOS thin film prepared by the present invention；
Fig. 3 is the transmitted spectrum figure that the present invention grows the BeZnOS thin film of preparation under different oxygen press strip parts.
Detailed description of the invention
Hereinafter principles of the invention and feature being described, illustrated embodiment is served only for explaining the present invention, is not intended to limit the scope of the present invention.
Embodiment 1
ZnS:BeO=95:5 weighs ZnS powder 18.5193 grams and 2.5012 grams of BeO powder in molar ratio, adds 13 grams of ball millings of deionized water 4 hours, afterwards at 110 DEG C of vacuum dryings after mixing.Dried powder adds tabletting after 2 grams of ethanol are fully ground stirring and becomes the circular blank of diameter 27.5mm, thickness 2mm.Blank is put into crucible and is placed in vacuum tube furnace, and is putting the identical powder of composition (5.0000 grams), high purity sulphur powder (1.1000 grams) about.High-purity argon gas is passed into after vacuum tube furnace is evacuated to 0.1Pa.Under protective atmosphere, tube furnace it is warming up to 1300 DEG C and is incubated 2 hours, naturally cooling to room temperature subsequently, obtain required ceramic target.Using this ceramic target as laser ablation target, and load vacuum chamber together with the ultrasonic cleaning substrate of 15 minutes respectively such as acetone, dehydrated alcohol and deionized water, and be evacuated to 10-4Pa.Open silicon and to regulate underlayer temperature be 750 DEG C.Pass into oxygen so that air pressure maintains 2Pa in whole film deposition process.Open substrate and target platform rotation.Setting laser instrument output energy as 350mJ/pulse, pulse recurrence frequency is 5Hz.Open laser deposition close oxygen after 30 minutes and stop silicon.Sample takes out vacuum chamber after naturally cooling to room temperature in a vacuum.The BeZnOS quaternary compound semiconductor thin-film material prepared for the present embodiment carries out XRD and the test of x-ray photoelectron power spectrum, and test result is as depicted in figs. 1 and 2.From figure 1 it appears that the XRD figure spectrum of this material only has the diffraction maximum of BeZnOS (002) and (004) crystal face, it was demonstrated that obtain the BeZnOS thin film of the high C-axis preferred orientation of pure buergerite phase；The x-ray photoelectron energy spectrogram of Fig. 2 occurs in that the characteristic peak of tetra-kinds of elements of Be, Zn, O and S, it was demonstrated that containing these four element in prepared thin film.
Embodiment 2
ZnS:BeO=85:15 weighs ZnS powder 16.5700 grams and 7.5036 grams of BeO powder in molar ratio, adds 12 grams of ball millings of deionized water 4 hours, afterwards at 110 DEG C of vacuum dryings after mixing.Dried powder adds tabletting after 2 grams of ethanol are fully ground stirring and becomes the circular blank of diameter 27.5mm, thickness 2.5mm.Blank is put into crucible and is placed in vacuum tube furnace, and is putting the identical powder of composition, high purity sulphur powder about.High-purity argon gas is passed into after vacuum tube furnace is evacuated to 0.1Pa.Under protective atmosphere, tube furnace it is warming up to 1100 DEG C and is incubated 5 hours, naturally cooling to room temperature subsequently, obtain required ceramic target.Using this ceramic target as laser ablation target, and load vacuum chamber together with the ultrasonic waves for cleaning substrate of 15 minutes respectively such as acetone, dehydrated alcohol and deionized water, and be evacuated to 10-4Pa.Open silicon and to regulate underlayer temperature be 700 DEG C.Pass into oxygen so that air pressure maintains 2Pa in whole film deposition process.Open substrate and target platform rotation.Setting laser instrument output energy as 450mJ/pulse, pulse recurrence frequency is 5Hz.Open laser deposition close oxygen after 40 minutes and stop silicon.Sample takes out vacuum chamber after naturally cooling to room temperature in a vacuum.
Embodiment 3
ZnS:BeO=92:8 weighs ZnS powder 17.9345 grams and 6.0216 grams of BeO powder in molar ratio, adds 24 grams of ball millings of deionized water 4 hours, afterwards at 110 DEG C of vacuum dryings after mixing.Dried powder adds tabletting after 2 grams of ethanol are fully ground stirring and becomes the circular blank of diameter 27.5mm, thickness 3mm.Blank is put into crucible and is placed in vacuum tube furnace, and is putting the identical powder of composition, high purity sulphur powder about.High-purity argon gas is passed into after vacuum tube furnace is evacuated to 0.1Pa.Under protective atmosphere, tube furnace it is warming up to 750 DEG C and is incubated 6 hours, naturally cooling to room temperature subsequently, obtain required ceramic target.Using this ceramic target as laser ablation target, and load vacuum chamber together with the ultrasonic waves for cleaning substrate of 15 minutes respectively such as acetone, dehydrated alcohol and deionized water, and be evacuated to 10-4Pa.Open silicon and to regulate underlayer temperature be 750 DEG C.Open substrate and target platform rotation.Pass into oxygen so that air pressure remains constant in whole film deposition process: oxygen press strip part respectively 0.05Pa, 1.0Pa and 2.0Pa, to prepare the BeZnOS thin-film material of different S content.Opening sample stage rotating speed is 10 revs/min, target platform rotation 5 revs/min.Setting laser instrument as permanent energy pattern, output energy is 300mJ/pulse, and pulse recurrence frequency is 5Hz, pulse number 9000.Open laser deposition close oxygen after 30 minutes and stop silicon.Sample takes out vacuum chamber after naturally cooling to room temperature in a vacuum.
The present embodiment prepared BeZnOS quaternary compound semiconductor thin-film material under different oxygen press strip part (0Pa, 0.1Pa and 6.0Pa) is carried out transmitted spectrum test, and result is as shown in Figure 3.As seen from the figure, along with the rising of oxygen pressure, the ABSORPTION EDGE of BeZnOS thin film occurs mobile, illustrates to realize the adjustment to thin film band gap.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all within the spirit and principles in the present invention, any amendment of making, equivalent replacement, improvement etc., should be included within protection scope of the present invention.
Claims (6)
1. the preparation method of a BeZnOS compound semiconductor materials, it is characterised in that comprise the following steps:
1) ceramic target needed for BeZnOS compound semiconductor film material is prepared, described ceramic target is obtained by ceramic green sheet sintering, wherein, described ceramic green sheet includes ZnS and the BeO that mol ratio is 99:1～70:30, the sintering temperature of described ceramic green sheet is 700～1250 DEG C, and sintering time is 4～6 hours；
2) with sapphire for substrate, pulsed laser ablation deposition method is adopted to carry out the growth of BeZnOS thin film over the substrate described ceramic target, obtain BeZnOS compound semiconductor materials, wherein, underlayer temperature is 25～1000 DEG C, laser energy is 250～600mJ/pulse, and oxygen pressure is 0～10Pa.
2. the preparation method of BeZnOS compound semiconductor materials according to claim 1, it is characterised in that described step 1) comprise the following steps:
1.1) weigh ZnS powder and BeO powder that mol ratio is 99:1～70:30, obtain just mixed powder；
1.2) to step 1.1) deionized water that adds just mixed powder gross mass 50～70% in the first mixed powder that obtains carries out ball milling, obtains mixed-powder；
1.3) by step 1.2) mixed-powder that obtains carries out vacuum drying treatment, obtains the mixed-powder dried, and wherein, background pressure≤0.1Pa, baking temperature is 100～120 DEG C, and drying time is 6～8 hours；
1.4) to step 1.3) the dry mixed-powder that obtains adds the dehydrated alcohol of dry mixed-powder gross mass 2～6%, grinding stirs, and obtains mixing the ceramic batch being bonded together；
1.5) by step 1.4) ceramic batch that obtains is pressed into ceramic green sheet, and the thickness of ceramic green sheet is 2～3mm；
1.6) with sulfur powder for oxygen scavenger, with argon for protection gas, to step 1.5 in vacuum tube furnace) ceramic green sheet that obtains is sintered, and obtains ceramic target.
3. the preparation method of BeZnOS compound semiconductor materials according to claim 1 and 2, it is characterised in that described step 2) comprise the following steps:
2.1) substrate grown as thin film using sapphire, and substrate is carried out ultrasonic waves for cleaning and dry, obtain clean substrate, wherein, cleanout fluid is any one or a few the mixing in acetone, dehydrated alcohol and deionized water, and scavenging period is 10～20 minutes；
2.2) under the atmospheric condition of oxygen, to step 1) ceramic target that obtains adopts pulsed laser ablation deposition method in step 2.1) the clean substrate that obtains carries out the growth of BeZnOS thin film.
4. a BeZnOS compound semiconductor materials, it is characterised in that for the quaternary compound semiconductor material that BeO and ZnS solid solution obtains.
5. BeZnOS compound semiconductor materials according to claim 4, it is characterised in that prepared by the arbitrary described preparation method of claims 1 to 3.
6. the application of the BeZnOS compound semiconductor materials according to claim 4 or 5, it is characterised in that as the active layer of the abarrier layer material of zno-based quantum well devices or ultraviolet light detector.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108396288A (en) * | 2018-03-30 | 2018-08-14 | 湖北大学 | Ultra-wide forbidden band ZrxSn1-xO2Alloy semiconductor epitaxial thin film material and preparation method thereof, application and device |
| CN109560162A (en) * | 2018-12-06 | 2019-04-02 | 湖北大学 | A kind of photodetector and preparation method thereof based on the nonpolar face a ZnOS film |
| CN109560150A (en) * | 2018-12-06 | 2019-04-02 | 湖北大学 | A kind of non-P-N junction type transparent membrane solar battery of the face m BeZnOS base and preparation method thereof |
| CN109560161A (en) * | 2018-12-06 | 2019-04-02 | 湖北大学 | Spontaneous polarization enhanced photodetector and preparation method thereof based on the face m ZnOS film |
| CN109585591A (en) * | 2018-12-06 | 2019-04-05 | 湖北大学 | A kind of MSM ultraviolet light detector and preparation method thereof based on non-polar plane type BeZnOS alloy crystal |
| CN109585593A (en) * | 2018-12-06 | 2019-04-05 | 湖北大学 | A kind of spontaneous polarization field enhanced ultraviolet optical detector and preparation method thereof based on BeZnOS quaternary alloy |
| CN109599449A (en) * | 2018-12-06 | 2019-04-09 | 湖北大学 | One kind is based on non-polar m face BeMgZnO transparent membrane solar battery and preparation method thereof |
| WO2020186767A1 (en) * | 2019-03-18 | 2020-09-24 | Shenzhen University | Composite-phase mechanoluminescent materials with adjustable color and intensity, and preparation method thereof |
| CN112195438A (en) * | 2020-09-10 | 2021-01-08 | 湖北大学 | Nitrogen-doped p-type transparent conductive BeZnOS film and preparation method and application thereof |
| CN112201711A (en) * | 2020-09-10 | 2021-01-08 | 湖北大学 | ZnO-based homojunction self-driven ultraviolet photoelectric detector and preparation method thereof |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108396288A (en) * | 2018-03-30 | 2018-08-14 | 湖北大学 | Ultra-wide forbidden band ZrxSn1-xO2Alloy semiconductor epitaxial thin film material and preparation method thereof, application and device |
| CN109560162A (en) * | 2018-12-06 | 2019-04-02 | 湖北大学 | A kind of photodetector and preparation method thereof based on the nonpolar face a ZnOS film |
| CN109560150A (en) * | 2018-12-06 | 2019-04-02 | 湖北大学 | A kind of non-P-N junction type transparent membrane solar battery of the face m BeZnOS base and preparation method thereof |
| CN109560161A (en) * | 2018-12-06 | 2019-04-02 | 湖北大学 | Spontaneous polarization enhanced photodetector and preparation method thereof based on the face m ZnOS film |
| CN109585591A (en) * | 2018-12-06 | 2019-04-05 | 湖北大学 | A kind of MSM ultraviolet light detector and preparation method thereof based on non-polar plane type BeZnOS alloy crystal |
| CN109585593A (en) * | 2018-12-06 | 2019-04-05 | 湖北大学 | A kind of spontaneous polarization field enhanced ultraviolet optical detector and preparation method thereof based on BeZnOS quaternary alloy |
| CN109599449A (en) * | 2018-12-06 | 2019-04-09 | 湖北大学 | One kind is based on non-polar m face BeMgZnO transparent membrane solar battery and preparation method thereof |
| CN109560150B (en) * | 2018-12-06 | 2020-03-24 | 湖北大学 | M-surface BeZnOS-based non-P-N junction type transparent thin-film solar cell and preparation method thereof |
| CN109599449B (en) * | 2018-12-06 | 2020-03-24 | 湖北大学 | Non-polar m-plane-based BeMgZnO transparent thin-film solar cell and preparation method thereof |
| CN109585591B (en) * | 2018-12-06 | 2020-04-03 | 湖北大学 | Non-polar surface type BeZnOS alloy crystal base MSM ultraviolet light detector and preparation method thereof |
| CN109560161B (en) * | 2018-12-06 | 2020-04-28 | 湖北大学 | Spontaneous polarization enhanced photoelectric detector based on m-plane ZnOS film and preparation method thereof |
| CN109560162B (en) * | 2018-12-06 | 2020-04-28 | 湖北大学 | Photoelectric detector based on nonpolar a-surface ZnOS film and preparation method thereof |
| WO2020186767A1 (en) * | 2019-03-18 | 2020-09-24 | Shenzhen University | Composite-phase mechanoluminescent materials with adjustable color and intensity, and preparation method thereof |
| CN112195438A (en) * | 2020-09-10 | 2021-01-08 | 湖北大学 | Nitrogen-doped p-type transparent conductive BeZnOS film and preparation method and application thereof |
| CN112201711A (en) * | 2020-09-10 | 2021-01-08 | 湖北大学 | ZnO-based homojunction self-driven ultraviolet photoelectric detector and preparation method thereof |
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Application publication date: 20160706 |