CN108251798A - A kind of preparation method of overlength zinc oxide micrometer line - Google Patents
A kind of preparation method of overlength zinc oxide micrometer line Download PDFInfo
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- CN108251798A CN108251798A CN201810033838.9A CN201810033838A CN108251798A CN 108251798 A CN108251798 A CN 108251798A CN 201810033838 A CN201810033838 A CN 201810033838A CN 108251798 A CN108251798 A CN 108251798A
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- zinc
- overlength
- zinc oxide
- micrometer line
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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
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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
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/407—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
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- Materials Engineering (AREA)
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- Metallurgy (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Physical Vapour Deposition (AREA)
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Abstract
The present invention relates to zinc oxide micrometer line preparation method technical fields, provide a kind of preparation method of overlength zinc oxide micrometer line, zinc-oxide film is prepared on a silicon substrate including the use of the method for magnetron sputtering；Then oxide powder and zinc, carbon dust and GaAs, are placed on as reaction source in ceramic boat；Silicon substrate is placed on the partial below along airflow direction of reaction source；Ceramic boat is placed in clean quartz ampoule, then quartz ampoule is placed on to the vitellarium of horizontal pipe furnace；By the use of argon gas as protection gas, overlength zinc oxide micrometer line is made after heating up, keeping the temperature, cool down.Whereby, the present invention prepares seed layer of the very thin zinc-oxide film as developing zinc oxide micro wire on a silicon substrate by using the method for magnetron sputtering, then grows the overlength zinc oxide micrometer line that section is quadrangle with the method for chemical vapor deposition.The pattern of micro wire is uniform, and section is tetrahedron, and length is more advantageous to manual operation up to 12 centimetres.The method of the present invention is at low cost and with repeatability well.
Description
Technical field
The present invention relates to zinc oxide micrometer line preparation method technical field more particularly to a kind of overlength zinc oxide micrometer lines
Preparation method.
Background technology
At present semi-conducting material light emitting diode, detector, solar cell, photocatalysis, gas sensor, etc. fields
It is widely used.Zinc oxide (ZnO) is II-VI group direct band-gap semicondictor, energy gap 3.37eV, the exciton knot of room temperature
60meV can be up to by closing, and be realize efficient ultraviolet excitonic luminescence at room temperature and laser one much larger than room temperature thermal energy (26meV)
Kind candidate material, and ZnO also has the features such as abundant raw materials, safety and environmental protection.
External (patent No. APPLIED PHYSICS LETTERS 92,2411022008), which is disclosed, a kind of utilizes thermal evaporation
Mode on ZnO/C targets (mass ratio 1:1) method of ZnO micro wires is directly grown, the section of obtained micro wire is six
Side shape.In addition, there is the method that some seminar utilize chemical vapor deposition, using carbon dust and oxide powder and zinc, (mass ratio is 1:1)
It is grown for raw material with the ZnO micro wires that section is six face shapes.
But micro wire is grown on ZnO/C targets using the mode of thermal evaporation, and for chemical vapor deposition method, mistake
Journey is complicated, of high cost.On the other hand, the length of micro wire prepared by the chemical vapor deposition reported arrives several at tens microns
The magnitude of millimeter to further make photoelectric device, needs to be operated by expensive precision instrument.
In summary, the existing technology has inconveniences and defects in actual use, so it is necessary to be improved.
Invention content
For it is above-mentioned the defects of, the purpose of the present invention is to provide a kind of preparation method of overlength zinc oxide micrometer line, lead to
It crosses and seed crystal of the very thin zinc-oxide film as developing zinc oxide micro wire is prepared using the method for magnetron sputtering on a silicon substrate
Layer, then grow the overlength zinc oxide micrometer line that section is quadrangle with the method for chemical vapor deposition.The pattern of micro wire is uniform,
Section is tetrahedron, and length is more advantageous to manual operation up to 1-2 centimetres.The method of the present invention is at low cost and with fine
Repeatability.
To achieve these goals, the present invention provides a kind of preparation method of overlength zinc oxide micrometer line, including walking as follows
Suddenly：
The first step：High pure metal Zn and high purity oxygen gas are selected as growth source, using the method for magnetron sputtering in silicon substrate
On prepare zinc-oxide film；
Growth parameter(s) is：400 DEG C of growth temperature, growth room vacuum degree 1Pa, 20 turns/min of sample stage rotating speed, radio frequency source work(
Rate 130W, growth time 1 hour；
Gas flow：Argon gas is 30sccm, oxygen 10sccm；
Second step：Oxide powder and zinc, carbon dust and GaAs are uniformly mixed by grinding obtained powder for a long time, as anti-
Ying Yuan is placed in ceramic boat；And by the silicon substrate made from the first step with zinc-oxide film be placed on the reaction source along air-flow
The partial below in direction；Then the ceramic boat is placed in clean quartz ampoule, then quartz ampoule is placed on horizontal pipe furnace
Vitellarium；Under normal pressure, with the speed heat temperature raising of 24 DEG C/min；At 950~1050 DEG C, 30 minutes are kept the temperature, then automatic drop
Temperature is until room temperature；Obtain the overlength zinc oxide micrometer line；
High-purity argon gas is persistently connected in entire heating, heat preservation, temperature-fall period as protection gas；
The purity ＞ 99.99% of the oxide powder and zinc；The mass ratio of the oxide powder and zinc, carbon dust and GaAs is 1：1：
0.1。
The preparation method of overlength zinc oxide micrometer line according to the present invention, the throughput of the high-purity argon gas is 100SCCM.
The preparation method of overlength zinc oxide micrometer line according to the present invention, the section of the overlength zinc oxide micrometer line is four
Side shape.
The preparation method of overlength zinc oxide micrometer line according to the present invention, the length of the overlength zinc oxide micrometer line are
1.0~2.0cm.
The purpose of the present invention is to provide a kind of preparation method of overlength zinc oxide micrometer line, by using magnetron sputtering
Method prepares seed layer of the very thin zinc-oxide film as developing zinc oxide micro wire on a silicon substrate, then uses chemical vapor deposition
Long-pending method growth section is the overlength zinc oxide micrometer line of quadrangle.The pattern of micro wire is uniform, and section is tetrahedron, length
Degree is more advantageous to manual operation up to 1-2 centimetres.The method of the present invention is at low cost and with repeatability well.
Description of the drawings
Fig. 1 is 5k times of scanning electron microscope (SEM) photograph of amplification of the zinc oxide micrometer line of the present invention.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
The present invention provides a kind of preparation method of overlength zinc oxide micrometer line, includes the following steps：
The first step：High pure metal Zn and high purity oxygen gas are selected as growth source, using the method for magnetron sputtering in silicon substrate
On prepare zinc-oxide film；
Growth parameter(s) is：400 DEG C of growth temperature, growth room vacuum degree 1Pa, 20 turns/min of sample stage rotating speed, radio frequency source work(
Rate 130W, growth time 1 hour.Gas flow：Argon gas is 30sccm, oxygen 10sccm；
Second step：Oxide powder and zinc, carbon dust and GaAs are uniformly mixed by grinding obtained powder for a long time, as anti-
Ying Yuan is placed in ceramic boat；And by the silicon substrate made from the first step with zinc-oxide film be placed on reaction source along airflow direction
Partial below；Then ceramic boat is placed in clean quartz ampoule, then quartz ampoule is placed on to the vitellarium of horizontal pipe furnace；
Under normal pressure, with the speed heat temperature raising of 24 DEG C/min；At 950~1050 DEG C, 30 minutes are kept the temperature, then automatic cooling is until room
Temperature；Obtain the overlength zinc oxide micrometer line；
High-purity argon gas is persistently connected in entire heating, heat preservation, temperature-fall period as protection gas；The high-purity argon gas
Throughput is 100SCCM；
The purity ＞ 99.99% of the oxide powder and zinc；The mass ratio of the oxide powder and zinc, carbon dust and GaAs is 1：1：
0.1；
Referring to Fig. 1, the section of the overlength zinc oxide micrometer line of the invention is quadrangle；
Using preceding method, only change the holding temperature in the second step, after cooling, the overlength oxygen of different length is made
Change zinc micro wire；Which part embodiment is as follows：
Embodiment one：
The second step cools down automatically after keeping the temperature 30 minutes at 960 DEG C until room temperature；Obtain the overlength zinc oxide micrometer line
Length be 1-2cm；
Embodiment two：
The second step cools down automatically after keeping the temperature 30 minutes at 1000 DEG C until room temperature；Obtain the overlength zinc oxide micrometer line
Length be 1-2cm；
Embodiment three：
The second step cools down automatically after keeping the temperature 30 minutes at 1030 DEG C until room temperature；Obtain the overlength zinc oxide micrometer line
Length be 1-2cm；
Example IV：
The second step cools down automatically after keeping the temperature 30 minutes at 1050 DEG C until room temperature；Obtain the overlength zinc oxide micrometer line
Length be 1-2cm；
Other embodiments repeat no more, it follows that when holding temperature is 950~1050 DEG C, overlength oxidation obtained
The length of zinc micro wire is 1.0~2.0cm.
In conclusion the purpose of the present invention is to provide a kind of preparation method of overlength zinc oxide micrometer line, by using
The method of magnetron sputtering prepares seed layer of the very thin zinc-oxide film as developing zinc oxide micro wire on a silicon substrate, then uses
The method growth section of chemical vapor deposition is the overlength zinc oxide micrometer line of quadrangle.The pattern of micro wire is uniform, and section is
Tetrahedron, length are more advantageous to manual operation up to 1-2 centimetres.The method of the present invention is at low cost and with repetition well
Property.
Certainly, the present invention can also have other various embodiments, without deviating from the spirit and substance of the present invention, ripe
It knows those skilled in the art and makes various corresponding changes and deformation, but these corresponding changes and change in accordance with the present invention
Shape should all belong to the protection domain of appended claims of the invention.
Claims (4)
1. a kind of preparation method of overlength zinc oxide micrometer line, which is characterized in that include the following steps：
The first step：High pure metal Zn and high purity oxygen gas is selected to be made on a silicon substrate using the method for magnetron sputtering as growth source
Standby zinc-oxide film；
Growth parameter(s) is：400 DEG C of growth temperature, growth room vacuum degree 1Pa, 20 turns/min of sample stage rotating speed, RF source power
130W, growth time 1 hour；
Gas flow：Argon gas is 30sccm, oxygen 10sccm；
Second step：Oxide powder and zinc, carbon dust and GaAs are uniformly mixed by grinding obtained powder for a long time, as reaction source
It is placed in ceramic boat；And by the silicon substrate made from the first step with zinc-oxide film be placed on the reaction source along airflow direction
Partial below；Then the ceramic boat is placed in clean quartz ampoule, then quartz ampoule is placed on to the growth of horizontal pipe furnace
Area；Under normal pressure, with the speed heat temperature raising of 24 DEG C/min；At 950~1050 DEG C, 30 minutes are kept the temperature, then automatic cooling is straight
To room temperature；Obtain the overlength zinc oxide micrometer line；
High-purity argon gas is persistently connected in entire heating, heat preservation, temperature-fall period as protection gas；
The purity ＞ 99.99% of the oxide powder and zinc；The mass ratio of the oxide powder and zinc, carbon dust and GaAs is 1：1：0.1.
2. the preparation method of overlength zinc oxide micrometer line according to claim 1, which is characterized in that the high-purity argon gas
Throughput is 100SCCM.
3. the preparation method of overlength zinc oxide micrometer line according to claim 1 or 2, which is characterized in that the overlength oxygen
The section for changing zinc micro wire is quadrangle.
4. the preparation method of overlength zinc oxide micrometer line according to claim 3, which is characterized in that the overlength zinc oxide
The length of micro wire is 1.0~2.0cm.
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| CN201810033838.9A CN108251798A (en) | 2018-01-15 | 2018-01-15 | A kind of preparation method of overlength zinc oxide micrometer line |
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| CN201810033838.9A CN108251798A (en) | 2018-01-15 | 2018-01-15 | A kind of preparation method of overlength zinc oxide micrometer line |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111029789A (en) * | 2019-12-24 | 2020-04-17 | 中国航空工业集团公司沈阳飞机设计研究所 | Wave-absorbing material with positive honeycomb structure of 10 degrees |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101319369A (en) * | 2008-04-15 | 2008-12-10 | 辽宁师范大学 | Method of preparing type p ZnO nano-wire |
-
2018
- 2018-01-15 CN CN201810033838.9A patent/CN108251798A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101319369A (en) * | 2008-04-15 | 2008-12-10 | 辽宁师范大学 | Method of preparing type p ZnO nano-wire |
Non-Patent Citations (1)
| Title |
|---|
| 丁梦: ""基于氧化锌微纳米线的光电器件研究"", 《中国博士学位论文全文数据库 信息科技辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111029789A (en) * | 2019-12-24 | 2020-04-17 | 中国航空工业集团公司沈阳飞机设计研究所 | Wave-absorbing material with positive honeycomb structure of 10 degrees |
| CN111029789B (en) * | 2019-12-24 | 2021-10-22 | 中国航空工业集团公司沈阳飞机设计研究所 | Wave-absorbing material with positive honeycomb structure of 10 degrees |
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Application publication date: 20180706 |