CN106086795B - A kind of zinc oxide/gallium nitride preparation method of composite film - Google Patents
A kind of zinc oxide/gallium nitride preparation method of composite film Download PDFInfo
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- CN106086795B CN106086795B CN201610377095.8A CN201610377095A CN106086795B CN 106086795 B CN106086795 B CN 106086795B CN 201610377095 A CN201610377095 A CN 201610377095A CN 106086795 B CN106086795 B CN 106086795B
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- zinc oxide
- gallium nitride
- laminated film
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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
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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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0617—AIII BV compounds, where A is Al, Ga, In or Tl and B is N, P, As, Sb or Bi
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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
- C23C14/06—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
Abstract
The invention discloses a kind of zinc oxide/gallium nitride laminated film preparation methods, using preparing zinc oxide/gallium nitride laminated film under pulsed laser deposition low temperature, the preparation method of ZnO-GaN composite material is not only expanded, the visible absorption higher than 600nm may be implemented, and compared with powder, the ZnO/GaN laminated film prepared on substrate is easier to reuse.Film particle diameter distribution prepared by the present invention is uniform, has apparent visible light-responded, and band gap reaches 1.6eV.
Description
Technical field
The invention belongs to photocatalysis technology fields, and in particular to a kind of preparation method of zinc oxide/gallium nitride laminated film.
Background technique
With the development of society, demand of the mankind to the energy is constantly increasing, bring energy crisis and ring therefrom
Border problem is the most pressing problem that we are faced.Hydrogen Energy is a kind of reproducible secondary energy sources, has cleaning, energy density
Height, thermal conductivity is good, reaction speed is fast and stores the advantages that diversified.It is generally used to the semiconductor as PhotoelectrochemicalSystem System for Hydrogen Production battery
Material has TiO2、ZnO、SrTiO3, (Adeli, B.and F.Taghipour, A the Review of such as SiC, GaN, CdS
Synthesis Techniques for Gallium-Zinc Oxynitride Solar-Activated
Photocatalyst for Water Splitting.Ecs Journal of Solid State Science and
Technology,2013.2(7):118-126.).However, that there is band gap is bigger (general big for most semiconductor materials
In 3eV) the shortcomings that, the ultraviolet light of sunshine gross energy 4% or so can only be utilized, how the efficient semiconductor light of development stability is urged
Change material, the visible light part of solar radiation can be utilized, become the hot spot of Recent study.
ZnO and GaN is direct band-gap semicondictor material, their crystal structures having the same and similar forbidden bandwidth
(ZnO forbidden bandwidth 3.37eV at room temperature, GaN at room temperature forbidden bandwidth 3.4eV), ZnO and GaN have excellent photoelectricity, piezoelectricity
With the performances such as photocatalysis, in ultraviolet detector, shine and laser device, solar battery, photocatalysis hydrogen production etc. have extensively
General application prospect.After the development of many years, the research of ZnO and GaN semiconductor material is in film growth, impurity regulation and device
Using etc. research obtain huge progress.Redox electricity of the conduction band and valence-band edge of ZnO and GaN across hydrolysis
Gesture meets the condition of optical electro-chemistry hydrolysis hydrogen.But since its forbidden bandwidth is wider, there is too in photocatalysis hydrogen production process
The disadvantages such as sunlight utilization is poor, quantum efficiency is low.
2005, ZnO and GaN were compounded to form ZnO-GaN solid solution by Maeda et al., it is found that it is a kind of with visible
Photoresponse can be used as the novel photocatalyst of photolysis water hydrogen, thus the new neck of one for opening photocatalysis hydrogen production investigation of materials
Domain (Maeda, K., et al., GaN:ZnO solid solution as a photocatalyst for visible-
light-driven overall water splitting.Journal of the American Chemical
Society,2005.127(23):p.8286-8287.).The method for being used to prepare ZnO-GaN solid solution at present is mainly high temperature
Solid-phase synthesis, the product prepared be powder, be not easy to collect and reuse (Ward, M.J., et al.,
Nitridation Temperature Effects on Electronic and Chemical Properties of(Ga1– xZnx)(N1–xOx)Solid Solution Nanocrystals.The Journal of Physical Chemistry C,
2013.117(39):p.20332-20342.)。
Summary of the invention
Goal of the invention: it is an object of the invention to provide a kind of preparation methods of butterfly-like copper hydroxyphosphate catalyst.
Technical solution: a kind of preparation method of zinc oxide/gallium nitride laminated film is prepared using pulsed laser deposition,
Target uses high-purity zinc oxide and gallium nitride, is loaded on the target pallet at 30 degree of angles respectively, between target and substrate
Distance be maintained at 7cm, specifically include the following steps:
1) substrate cleans, with being put into vacuum chamber after being dried with nitrogen,
2) vacuumizing so that the vacuum degree of settling chamber reaches 5 × 10-7Torr using mechanical pump and molecular pump, is passed through height
Pure nitrogen gas, gas flow 30sccm, standing a period of time to deposit indoor vacustat to be 1.2 × 10-2Torr,
3) pre-deposition, substrate are blocked using demarcation plate, are bombarded in advance with laser zinc oxide and gallium nitride target,
4) laser first bombards zinc oxide target 25 times, then switches to gallium nitride target and bombards 25 times, so follows for one
Ring, repetitive cycling 300 times,
5) zinc oxide/gallium nitride laminated film is obtained after being passed through high pure nitrogen cooling, the laminated film thickness of deposition is about
200nm。
Further, the substrate is Sapphire Substrate, because Sapphire Substrate and zinc oxide and gallium nitride have it is lesser
Lattice be excuse me, but I must be leaving now.
Further, the cleaning process in step 1) is by Sapphire Substrate respectively in acetone, dehydrated alcohol and deionization
It is cleaned by ultrasonic 15 minutes in water.
Further, the optical maser wavelength in step 3) and step 4) when laser bombardment target is 248nm, energy 220mJ,
Frequency is 3Hz.
Further, in step 4), target and substrate are rotated with 20 revs/min of rate, the purpose is to make by
The target of bombardment and the film being deposited on substrate are more evenly.
Further, high pure nitrogen is passed through in step 5) makes the pressure in vacuum chamber be maintained at 1 × 104Torr。
The utility model has the advantages that the present invention is using pulsed laser deposition, low temperature preparation ZnO and GaN is compound on a sapphire substrate
Film has not only expanded the preparation method of ZnO-GaN composite material, and the visible absorption higher than 600nm, Er Qiehe may be implemented
Powder is compared, and the ZnO/GaN laminated film prepared on substrate is easier to reuse.Film particle diameter distribution prepared by the present invention
Uniformly, have apparent visible light-responded, band gap reaches 1.6eV.
Detailed description of the invention
Fig. 1 is the scanning electron microscope image according to 1 product of embodiment.
Fig. 2 is the EDS power spectrum image according to 1 product of embodiment.
Fig. 3 is the transmission spectrum of 1 product of embodiment.
Fig. 4 is the transmission spectrum of 2 product of embodiment.
Specific embodiment
In order to deepen the understanding of the present invention, below in conjunction with embodiment and attached drawing, the invention will be further described, should
The examples are only for explaining the invention, is not intended to limit the scope of the present invention..
Embodiment 1
By Sapphire Substrate respectively in acetone, absolute ethanol and deionized water be cleaned by ultrasonic 15 minutes, after blown with nitrogen
It is dry, it is put into vacuum deposition chamber.Experiment uses pulsed laser deposition, and target uses high-purity zinc oxide and gallium nitride, respectively
It is loaded on the target pallet at 30 degree of angles.Using vacuumizing so that the vacuum degree of settling chamber reaches for mechanical pump and molecular pump
5×10-7Torr.It is passed through high pure nitrogen, gas flow 30sccm.It stands and to deposit indoor vacustat for a period of time
It is 1.2 × 10-2Torr.The underlayer temperature of deposition is room temperature (23 DEG C).Laser light source uses optical maser wavelength quasi- for the KrF of 248nm
Molecular laser, frequency 3Hz, laser energy 220mJ, laser are focused on target by external focus lamp.Target and lining
The distance between bottom is maintained at 7cm.Before formally preparing sample, preliminary sedimentation first is carried out to zinc oxide and gallium nitride target with laser
Product, substrate is blocked using demarcation plate when pre-deposition.When formal deposition, laser first bombards zinc oxide target 25 times, then switches to
Gallium nitride target bombards 25 times, is so a circulation, and repetitive cycling 300 times.Be passed through high pure nitrogen it is cooling after obtain zinc oxide/
Gallium nitride laminated film.
Fig. 1 is the zinc oxide/gallium nitride laminated film scanning electron microscope image prepared, as can be seen from the figure thin
The even particle distribution of film.
Fig. 2 is the zinc oxide/gallium nitride laminated film EDS energy spectrum diagram prepared, as can clearly see from the figure zinc and
The peak of gallium, wherein Sapphire Substrate is had at the peak of aluminium by oneself.
Fig. 3 is the zinc oxide/gallium nitride laminated film transmission spectrum prepared, as can be seen from the figure the ABSORPTION EDGE of its transmission
In 600nm or so, can obtain its band gap width by analysis is about 1.6eV.
Embodiment 2
Substrate deposition temperature in embodiment 1 is increased to 50 DEG C by room temperature (23 DEG C) and keeps this temperature during the deposition process
It spends constant.Fig. 4 is zinc oxide/gallium nitride laminated film transmission spectrum for preparing when underlayer temperature is 50 DEG C, can be with from figure
Find out its transmission ABSORPTION EDGE and compared apparent blue-shifted phenomenon at room temperature, illustrate increase depositing temperature improve zinc oxide/
The band gap of gallium nitride laminated film, can obtain its band gap width by analysis is about 1.7eV.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of zinc oxide/gallium nitride laminated film preparation method, which is characterized in that it is prepared using pulsed laser deposition,
Target uses high-purity zinc oxide and gallium nitride, is loaded on the target pallet at 30 degree of angles respectively, between target and substrate
Distance be maintained at 7cm, specifically include the following steps:
1) substrate cleans, with being put into vacuum chamber after being dried with nitrogen,
2) vacuumizing so that the vacuum degree of settling chamber reaches 5 × 10 using mechanical pump and molecular pump-7Torr is passed through High Purity Nitrogen
Gas, gas flow 30sccm, standing a period of time to deposit indoor vacustat to be 1.2 × 10-2Torr,
3) pre-deposition, substrate are blocked using demarcation plate, are bombarded in advance with laser zinc oxide and gallium nitride target,
4) laser first bombards zinc oxide target 25 times, then switches to gallium nitride target and bombards 25 times, is so a circulation, weight
It recycles 300 times again,
5) zinc oxide/gallium nitride laminated film is obtained after being passed through high pure nitrogen cooling.
2. zinc oxide according to claim 1/gallium nitride laminated film preparation method, which is characterized in that the substrate
For Sapphire Substrate.
3. zinc oxide according to claim 1/gallium nitride laminated film preparation method, which is characterized in that in step 1)
Cleaning process be by Sapphire Substrate respectively in acetone, absolute ethanol and deionized water be cleaned by ultrasonic 15 minutes.
4. zinc oxide according to claim 1/gallium nitride laminated film preparation method, which is characterized in that step 3) and
Optical maser wavelength in step 4) when laser bombardment target is 248nm, energy 220mJ, frequency 3Hz.
5. zinc oxide according to claim 1/gallium nitride laminated film preparation method, which is characterized in that in step 4),
Target and substrate are rotated with 20 revs/min of rate.
6. zinc oxide according to claim 1/gallium nitride laminated film preparation method, which is characterized in that in step 5)
Being passed through high pure nitrogen makes the pressure in vacuum chamber be maintained at 1 × 104Torr。
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101728248A (en) * | 2008-10-15 | 2010-06-09 | 中国科学院半导体研究所 | Growing method of gallium nitride |
| CN101969091A (en) * | 2010-09-17 | 2011-02-09 | 武汉迪源光电科技有限公司 | Light emitting diode |
| CN101976800A (en) * | 2010-10-09 | 2011-02-16 | 吉林大学 | ZnO and GaN-combined ZnO-based end surface transmitting laser and preparation method thereof |
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- 2016-05-31 CN CN201610377095.8A patent/CN106086795B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101728248A (en) * | 2008-10-15 | 2010-06-09 | 中国科学院半导体研究所 | Growing method of gallium nitride |
| CN101969091A (en) * | 2010-09-17 | 2011-02-09 | 武汉迪源光电科技有限公司 | Light emitting diode |
| CN101976800A (en) * | 2010-10-09 | 2011-02-16 | 吉林大学 | ZnO and GaN-combined ZnO-based end surface transmitting laser and preparation method thereof |
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Address after: Room 420, block C, Kechuang headquarters building, No. 320, pubin Road, Jiangpu street, Pukou District, Nanjing, Jiangsu Patentee after: NANJING University OF INFORMATION SCIENCE & TECHNOLOGY Address before: The Olympic Avenue in Jianye District of Nanjing city of Jiangsu Province, No. 69 210019 Patentee before: NANJING University OF INFORMATION SCIENCE & TECHNOLOGY |