CN105839055A - Method for preparation of one-dimensional-nanostructure zinc oxide by thin film deposition - Google Patents
Method for preparation of one-dimensional-nanostructure zinc oxide by thin film deposition Download PDFInfo
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- CN105839055A CN105839055A CN201610158232.9A CN201610158232A CN105839055A CN 105839055 A CN105839055 A CN 105839055A CN 201610158232 A CN201610158232 A CN 201610158232A CN 105839055 A CN105839055 A CN 105839055A
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- Prior art keywords
- target
- zinc
- substrate
- zinc oxide
- sputtering
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Classifications
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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 relates to a method for preparation of one-dimensional-nanostructure zinc oxide by thin film deposition, and belongs to the field of semiconductor materials. The method comprises the steps: zinc or zinc oxide with the purity of 99.99% is made into a target with the diameter of 1 inch and the thickness of 0.25 inch; a single crystal or glass is used as a substrate, and the substrate is subjected to ultrasonic cleaning, then is cleaned for 20 minutes in a cleaning solvent, rinsed with deionized water, and finally dried by nitrogen gas; the target and the substrate are put into a vacuum cavity of a pulsed laser deposition device; the initial pressure of the vacuum cavity is 2*10<-6> Torr, the oxygen pressure is set to 5 mTorr-50 Torr in a sputtering process, the temperature is from room temperature to 900 DEG C, the laser energy is 1-10 mJ/cm<2>, and the distance from the target to the substrate is 10-80 cm. Laser used by the method is clean and only applies heat to the surface of a material to be evaporated, and pollution from a heating source, a support and the like is reduced to the lowest level; the evaporation rate is high, the process is easy to control, the prepared one-dimensional-nanostructure zinc oxide not only has uniform length, width and morphology, and a compound deviation phenomenon cannot occur.
Description
Technical field
The present invention relates to a kind of method utilizing thin film deposition to prepare one-dimensional nanostructure zinc, belong to field of semiconductor materials.
Background technology
One-dimensional nano structure caused the broad interest of academia due to its unique superior performance in the last few years.According to pattern
Difference, one-dimensional nano structure is also designated as whisker, fiber, nano wire, nanometer rods, nano belt or nanotube.Make with them
The nanometer components and parts made can be widely applied to the fields such as nanoelectronics, photonic propulsion and overdelicate bimolecular sensors.
The semi-conducting material of tradition routine may be used for preparing one-dimensional nano structure.
Zinc oxide has the piezoelectricity of uniqueness, optically and mechanically characteristic and receives much concern.Use the nanometer unit that zinc oxide nanowire makes
Part can be used to develop nano generator and nano laser.Additionally, due to the specific surface area that zinc oxide nanowire is the biggest, also can quilt
As nanosensor device.
Zinc oxide nanowire can at high temperature prepare by direct evaporation Zinc oxide powder, such as thermal evaporation zinc oxide and the mixed powder of stone grinder
End, it is also possible to carry out in the vacuum container based on chemical vapour deposition technique, or can be with zinc chloride and hydrogen-oxygen in water
The hydro-thermal reaction changing sodium is made, and additionally prepared by available radio frequencies sputtering technology.The one-D nano zinc oxide prepared by vacuum evaporating technology
Not only the disunity such as Length x Width pattern is uneven, and real income product is compared with target product and component deviation can be occurred.
Summary of the invention
For above-mentioned technical problem, the present invention provides a kind of method utilizing thin film deposition to prepare one-dimensional nanostructure zinc, adopts
One-dimensional nanostructure zinc is prepared with pulsed laser deposition.By controlling sedimentary condition and parameter, control 1-dimention nano
The Length x Width of zinc oxide and pattern, be used for manufacturing the high-purity one-dimension zinc oxide nanostructured meeting actual application conditions and standard.
Concrete technical scheme is:
The method utilizing thin film deposition to prepare one-dimensional nanostructure zinc, comprises the following steps:
With the zinc that purity is 99.99% or zinc oxide, make diameter 1 inch, the target of thickness 0.25 inch；With monocrystalline or glass conduct
Substrate, after substrate ultrasonic waves for cleaning, cleans 20 minutes in cleaning solvent, then with deionized water rinsing, is finally dried with nitrogen；
Target and substrate are put in the vacuum chamber of pulsed laser deposition equipment；The initial pressure of vacuum chamber is 2 × 10-6Torr, sputter procedure
In oxygen pressure is set in 5 millitorrs～50 torr, temperature is room temperature～900 DEG C, and laser energy is 1～10 MJ every square centimeter, and target arrives
Substrate distance is 10～80 centimetres.
Concrete, before sputtering, first carrying out pre-sputtering, the entry material removing target guarantees the uniformity when formal sputtering；Sputtering
Time, first sputtering catalytic metal target, sputters zinc or zinc oxide target the most again；After sputtering, carry out being cooled to room temperature in nitrogen
Take out.
Described cleaning solvent is acetone, ethanol, isopropanol.
Described catalytic metal target is that Au Ag Pt Pd metal is made.
According to setting different experiment conditions and parameter, zinc oxide nanowire controlled diameter system is between 40 to 100 nanometers, and length can
To control more than 500 nanometers.
Pulsed laser deposition is typically used for preparing thin film or thick-film material, is rarely used for preparing the function oxidation of other structures
Thing.What the present invention provided utilizes the method that thin film deposition prepares one-dimensional nanostructure zinc, uses pulsed laser deposition system
Standby one-dimensional nanostructure zinc, owing to the laser of the method application is cleaning, and only applies material surface to be deposited
Heat, this just makes the pollution from heating source and supporter etc. be reduced to floor level；Evaporation rate is high, and process is easily controlled,
The one-D nano zinc oxide not only Length x Width pattern of preparation is uniform, and component deviation phenomenon will not occur.
Accompanying drawing explanation
Fig. 1 is the electron microscope observation finished product complexion figure of the embodiment of the present invention.
Detailed description of the invention
It is described in conjunction with the embodiments the detailed description of the invention of the present invention.
Embodiment 1
Using a diameter of 1 inch, thickness is 0.25 inch, and purity is the zinc oxide target of 99.99%, and monocrystal silicon is as substrate.Substrate
Being completed by ultrasonic cleaner, in acetone cleaning solvent, each cleaning 20 minutes, afterwards with deionized water rinsing, finally use nitrogen
It is dried.Putting into vacuum chamber, the initial pressure of vacuum chamber is 2 × 10-6Torr.Before formal sputtering, first carry out pre-sputtering, go
Entry material except target.First sputter the Metal Palladium of the gold system of 5 nano thickness, the zinc oxide of sputtering 1 micron subsequently.In sputter procedure
Arranging oxygen pressure is 500 millitorrs, and temperature is 500 degrees Celsius, and laser energy is 2 MJs every square centimeter, and target to substrate distance is
70 centimetres.After sputtering, cool down in nitrogen, decline per minute 6 degrees Celsius, until during room temperature, can take out.
Scanned electron microscope observation finished product complexion is shown as shown in Figure 1, i.e. zinc-oxide nano linear diameter is about 50 to 100 nanometers, long
Degree is about 1 micron.
Embodiment 2
Using a diameter of 1 inch, thickness is 0.25 inch, and purity is the zinc target of 99.99%, and monocrystal silicon is as substrate.Substrate is by surpassing
Sound wave washer completes, and in ethanol cleaning solvent, each cleaning 20 minutes, afterwards with deionized water rinsing, are finally dried with nitrogen.
Putting into vacuum chamber, the initial pressure of vacuum chamber is 2 × 10-6Torr.Before formal sputtering, first carry out pre-sputtering, remove target
Entry material.First sputter the Metal Palladium of the silvery of 5 nano thickness, the subsequently zinc of sputtering 1 micron.Sputter procedure arranges oxygen pressure
Power is 5 millitorrs, and temperature is 900 degrees Celsius, and laser energy is 1 MJ every square centimeter, and target to substrate distance is 10 centimetres.Sputtering
After, cool down in nitrogen, decline per minute 6 degrees Celsius, until during room temperature, can take out.
Embodiment 3
Using a diameter of 1 inch, thickness is 0.25 inch, and purity is the zinc target of 99.99%, and glass is as substrate.Substrate is by surpassing
Sound wave washer completes, each cleaning 20 minutes in isopropanol cleaning solvent, afterwards with deionized water rinsing, finally does with nitrogen
Dry.Putting into vacuum chamber, the initial pressure of vacuum chamber is 2 × 10-6Torr.Before formal sputtering, first carry out pre-sputtering, go
Entry material except target.First sputter the Metal Palladium of the platinum of 5 nano thickness, the subsequently zinc of sputtering 1 micron.Sputter procedure sets
Putting oxygen pressure is 50 torr, and temperature is room temperature, is generally defaulted as 25 degrees Celsius, and laser energy is 10 MJs every square centimeter,
Target is 80 centimetres to substrate distance.After sputtering, cool down in nitrogen, decline per minute 6 degrees Celsius, until room temperature
During left and right, can take out.
Claims (4)
1. utilize the method that one-dimensional nanostructure zinc is prepared in thin film deposition, it is characterised in that: comprise the following steps:
With the zinc that purity is 99.99% or zinc oxide, make diameter 1 inch, the target of thickness 0.25 inch；With monocrystalline or glass conduct
Substrate, after substrate ultrasonic waves for cleaning, cleans 20 minutes in cleaning solvent, then with deionized water rinsing, is finally dried with nitrogen；
Target and substrate are put in the vacuum chamber of pulsed laser deposition equipment；The initial pressure of vacuum chamber is 2 × 10-6Torr, sputter procedure
In oxygen pressure is set in 5 millitorrs～50 torr, temperature is room temperature～900 DEG C, and laser energy is 1～10 MJ every square centimeter, and target arrives
Substrate distance is 10～80 centimetres.
The method utilizing thin film deposition to prepare one-dimensional nanostructure zinc the most according to claim 1, it is characterised in that: spatter
Before penetrating, first carrying out pre-sputtering, the entry material removing target guarantees the uniformity when formal sputtering；
During sputtering, first sputtering catalytic metal target, sputters zinc or zinc oxide target the most again；After sputtering, carry out cold in nitrogen
But arrive room temperature to take out.
The method utilizing thin film deposition to prepare one-dimensional nanostructure zinc the most according to claim 1, it is characterised in that: institute
The cleaning solvent stated is acetone, ethanol, isopropanol.
The method utilizing thin film deposition to prepare one-dimensional nanostructure zinc the most according to claim 2, it is characterised in that:
Described catalytic metal target is that Au Ag Pt Pd metal is made.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610158232.9A CN105839055A (en) | 2016-03-21 | 2016-03-21 | Method for preparation of one-dimensional-nanostructure zinc oxide by thin film deposition |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610158232.9A CN105839055A (en) | 2016-03-21 | 2016-03-21 | Method for preparation of one-dimensional-nanostructure zinc oxide by thin film deposition |
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| CN105839055A true CN105839055A (en) | 2016-08-10 |
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| CN201610158232.9A Pending CN105839055A (en) | 2016-03-21 | 2016-03-21 | Method for preparation of one-dimensional-nanostructure zinc oxide by thin film deposition |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20090009510A (en) * | 2007-07-20 | 2009-01-23 | 이기원 | Manufacturing method of nano sized wire |
| US20090235862A1 (en) * | 2008-03-24 | 2009-09-24 | Samsung Electronics Co., Ltd. | Method of manufacturing zinc oxide nanowires |
| GB2469869A (en) * | 2009-05-01 | 2010-11-03 | Univ Bolton | Continuous ZnO films |
| CN102115339A (en) * | 2010-01-06 | 2011-07-06 | 济南大学 | Laser ablation growing method of zinc oxide nanowire array with controllable density |
-
2016
- 2016-03-21 CN CN201610158232.9A patent/CN105839055A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20090009510A (en) * | 2007-07-20 | 2009-01-23 | 이기원 | Manufacturing method of nano sized wire |
| US20090235862A1 (en) * | 2008-03-24 | 2009-09-24 | Samsung Electronics Co., Ltd. | Method of manufacturing zinc oxide nanowires |
| GB2469869A (en) * | 2009-05-01 | 2010-11-03 | Univ Bolton | Continuous ZnO films |
| CN102115339A (en) * | 2010-01-06 | 2011-07-06 | 济南大学 | Laser ablation growing method of zinc oxide nanowire array with controllable density |
Non-Patent Citations (3)
| Title |
|---|
| A. MARCU等: "Catalyst size limitation in vapor–liquid–solid ZnO nanowire growth using pulsed laser deposition", 《THIN SOLID FILMS》 * |
| HYO JEONG SON等: "Synthesis of ZnO nanowires by pulsed laser deposition in furnace", 《APPLIED SURFACE SCIENCE》 * |
| 刘志海等: "《加工玻璃生产操作问答》", 30 September 2009, 北京：化学工业出版社 * |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
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| TA01 | Transfer of patent application right |
Effective date of registration: 20171108 Address after: 1043 room 10, building 2, 455, Hubei Road, Urumqi, Urumqi economic and Technological Development Zone, the Xinjiang Uygur Autonomous Region, Kanas, 830011 Applicant after: Urumqi new Mstar Technology Ltd Address before: 300170, Hedong District, Tianjin Blue Garden 11 floor, 3 doors, 4 layers Applicant before: Wang Ye |
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| TA01 | Transfer of patent application right | ||
| CI02 | Correction of invention patent application |
Correction item: Applicant|Address Correct: Urumqi Xikesikexin Mstar Technology Ltd|1043 room 10, building 2, 455, Hubei Road, Urumqi, Urumqi economic and Technological Development Zone, the Xinjiang Uygur Autonomous Region, Kanas, 830011 False: Urumqi new Mstar Technology Ltd|1043 room 10, building 2, 455, Hubei Road, Urumqi, Urumqi economic and Technological Development Zone, the Xinjiang Uygur Autonomous Region, Kanas, 830011 Number: 48-01 Volume: 33 |
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| CI02 | Correction of invention patent application | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20160810 |
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| WD01 | Invention patent application deemed withdrawn after publication |