CN110735109A - nanometer zinc oxide with indium element adulterant - Google Patents
nanometer zinc oxide with indium element adulterant Download PDFInfo
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- CN110735109A CN110735109A CN201910912650.6A CN201910912650A CN110735109A CN 110735109 A CN110735109 A CN 110735109A CN 201910912650 A CN201910912650 A CN 201910912650A CN 110735109 A CN110735109 A CN 110735109A
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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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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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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
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive 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
- 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
- C23C14/3464—Sputtering using more than one target
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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
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
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Abstract
The invention discloses nanometer zinc oxide with indium element dopants, which comprises a zinc part with the weight percentage of more than 99 percent, a th indium element dopant part, a second cobalt element dopant part, and a copper element dopant part, wherein the th indium dopant part, the second cobalt element dopant part, and the copper element dopant part exist in a weight ratio of 1:1.5, the th indium element dopant part, the second cobalt element dopant part, and the copper element dopant part are doped into zinc oxide by adopting a radio frequency reactive sputtering method, and the zinc oxide prepared by the sputtering method is activated and processed into the nanometer zinc oxide doped with the indium element.
Description
Technical Field
The invention relates to kinds of nano zinc oxide with indium element adulterant.
Background
Nano-zinc oxide (nano-ZnO) is used as direct band gap wide bandgap semiconductor oxides, has a wider band gap (3.4 eV) and larger exciton binding energy (60MeV), so that series of excellent optical, electrical and magnetic properties are generated, and better plasticity and biocompatibility are added, so that the nano-zinc oxide has potential application values in the fields of manufacturing of optical devices and wave-absorbing materials, sewage treatment, biomedicine and the like.
The invention aims to prepare the indium-doped blue-light zinc oxide nano material with excellent performance by a radio frequency method.
Disclosure of Invention
The present invention aims at providing kinds of nanometer zinc oxide with indium element dopant to solve the said problems.
nanometer zinc oxide with indium element dopant, which comprises more than 99 wt% zinc part, indium element dopant part and second cobalt element, copper element dopant part;
the indium dopant moiety and the second cobalt and copper dopant moiety are present in a 1:1.5 weight ratio;
the indium element adulterant part, the second cobalt element adulterant part and the copper element adulterant part are doped into the zinc oxide by adopting a radio frequency reactive sputtering method, wherein the sputtering conditions are that the pre-vacuum before sputtering is 5-6 Pa, the substrate is a silicon single crystal, the diameter of the sputtering target is 10mm, the purity of the sputtering target is more than 99.99 percent, the sputtering reaction gas is the mixed gas of argon and oxygen, the distance between the substrate and the metal zinc target is 50mm, the substrate temperature is 100 ℃ and 300 ℃, the sputtering power is 60-200W, the sputtering pressure is 1-3.8 Pa, and the sputtering time is 1-2 h;
mixing zinc oxide prepared by a sputtering method with water to prepare a nano zinc oxide aqueous suspension with the mass concentration of 5.8%, ultrasonically dispersing for 4-6 minutes, adding aluminum potassium sulfate with the mass of 1.8% of that of the nano zinc oxide, adding the mixture into a high-speed stirrer, stirring for 1 hour at the rotating speed of 3200r/min, dripping a sodium hydroxide solution within 2-3 minutes, transferring the mixture into a reaction kettle lined with polytetrafluoroethylene, placing the reaction kettle into a homogeneous reactor, and reacting at the temperature of 100-120 ℃ for 6-8 hours; and after the reaction is finished, cooling to room temperature, performing centrifugal separation, washing and drying to obtain the indium-doped nano zinc oxide.
, arranging three groups of metal zinc targets, wherein indium sheets and cobalt sheets are uniformly arranged on the three groups of metal zinc targets respectively, the three groups of metal zinc targets are uniformly arranged around the silicon single crystal substrate, the indium sheets account for 3% of the metal zinc targets, the copper sheets account for 1.1-2.5% of the metal zinc targets, and the cobalt sheets account for 1% of the metal zinc targets.
And , cleaning and passivating the surface of the silicon single crystal substrate by plasma.
, adding silicon carbide to control the concentration of the dopant during the annealing process of preparing the nanometer zinc oxide doped with the indium element by the sputtering method of the radio frequency reaction.
The invention has the beneficial effects that: the crystalline phase of the nano zinc oxide analyzed by the X-ray diffractometer with the indium element dopant shows that the intensity of the diffraction peak of the nano zinc oxide with the indium element dopant is 3.5 times of that of the nano zinc oxide without doping, and simultaneously the crystal quality of the nano zinc oxide is effectively improved, and the specific excellent effects are as follows:
(1) the silicon single crystal substrate is cleaned and passivated by plasma, the balance of an oxide layer and interface charges on the surface of the substrate is solved,
(2) the defect concentration of oxygen vacancies in the zinc oxide hexagonal fiber structure is reduced by improving the concentration of oxygen in the sputtering reaction gas;
(3) the compensation of indium element and cobalt element on copper ion 1+ is utilized to reduce the influence of copper ion 1+ displacement and copper ion 2+ gap;
(4) the doping element and the zinc element are replaced to increase the concentration of gap filling defects of the doping element and the zinc element, and stronger blue-violet double peaks can be observed in a photoluminescence spectrum.
Detailed Description
In the specific embodiment 1, kinds of nano zinc oxide with indium element dopant comprises more than 99 wt% of zinc, th indium element dopant and second cobalt element and copper element dopant, th indium dopant and second cobalt element and copper element dopant exist according to a weight ratio of 1:1.5, th indium element dopant and second cobalt element and copper element dopant are doped into zinc oxide by a radio frequency reactive sputtering method, the sputtering conditions are that the pre-vacuum is 5-6 Pa before sputtering, the substrate is a silicon single crystal sputtering target, the diameter of the metal zinc target is 10mm, the purity is more than 99.99%, the sputtering reaction gas is mixed gas of argon and oxygen, the distance between the substrate and the metal zinc target is 50mm, the substrate temperature is 100 ℃, the power is 60-200W, the sputtering pressure is 1-3.8 Pa, the sputtering time is 1-2h, the metal zinc targets are provided with three groups, three groups of metal zinc targets are respectively and uniformly placed on the three groups of metal zinc targets, cobalt sheets are uniformly placed on the substrate, the substrate is cleaned by a cobalt sheet, the concentration of the silicon single crystal sputtering gas is 3-8 Pa after the silicon single crystal sputtering reaction target is uniformly stirred for 1-2h, the copper sheet is added into a silicon oxide substrate, the zinc oxide, the copper sheet is uniformly stirred, the copper sheet is added into a silicon substrate, the zinc oxide is stirred, the zinc oxide is stirred at a high-zinc oxide, the zinc oxide is stirred at room temperature of the zinc oxide, the zinc oxide is uniformly stirred, the zinc oxide is stirred, the zinc oxide is stirred at room temperature of the zinc oxide is stirred, the zinc oxide is uniformly stirred, the zinc oxide is stirred for 1-zinc oxide, the zinc oxide is stirred for 3.
In the specific embodiment 2, kinds of nano zinc oxide with indium element dopants comprises a zinc part, a th indium element dopant part, a second cobalt element dopant part, and a copper element dopant part, which are more than 99 wt%, a th indium dopant part, a second cobalt element dopant part, and a copper element dopant part exist according to a weight ratio of 1:1.5, a th indium element dopant part, a second cobalt element dopant part, and a copper element dopant part are doped into zinc oxide by a radio frequency reactive sputtering method, wherein the sputtering conditions include that a pre-vacuum is 5-6 Pa before sputtering, a substrate is a silicon single crystal sputtering target, a metal zinc target with a diameter of 10mm and a purity of more than 99.99%, a sputtering reaction gas is a mixed gas of argon and oxygen, a distance between the substrate and the metal zinc target is 50mm, a substrate temperature is 200 ℃, a sputtering power is 60-200W, a sputtering gas pressure is 1-3.8 Pa, a sputtering time is 1-2h, sputtering targets are provided with three groups of metal zinc targets, three groups of indium targets are respectively uniformly placed on the three groups of metal zinc targets, a cobalt sheets are uniformly placed on the substrate, a silicon single crystal sputtering pressure is 1-3.8 Pa sputtering target, a silicon single crystal sputtering reaction target is uniformly cleaned, a copper sheet is uniformly stirred, a copper sheet is added into a copper sheet, a copper sheet is uniformly stirred, a copper sheet is added into a copper sheet, a copper sheet is uniformly stirred, a copper sheet is added into a copper sheet.
In the specific embodiment 3, kinds of nano zinc oxide with indium element dopants comprises a zinc part, a th indium element dopant part, a second cobalt element dopant part, and a copper element dopant part, which are more than 99 wt%, a th indium dopant part, a second cobalt element dopant part, and a copper element dopant part exist according to a weight ratio of 1:1.5, a th indium element dopant part, a second cobalt element dopant part, and a copper element dopant part are doped into zinc oxide by a radio frequency reactive sputtering method, wherein the sputtering conditions include that a pre-vacuum is 5-6 Pa before sputtering, a substrate is a silicon single crystal sputtering target, a metal zinc target with a diameter of 10mm and a purity of more than 99.99%, a sputtering reaction gas is a mixed gas of argon and oxygen, a distance between the substrate and the metal zinc target is 50mm, a substrate temperature is 300 ℃, a sputtering power is 60-200W, a sputtering gas pressure is 1-3.8 Pa, a sputtering time is 1-2h, sputtering targets are respectively placed on the three groups of metal zinc targets, three groups of the substrate are uniformly placed on the cobalt sheets, a substrate, a silicon single crystal sputtering gas is cleaned at a sputtering pressure of 1-3.8 Pa, a silicon single crystal sputtering target, a silicon single crystal sputtering reaction target is uniformly stirred for 1-2h, a copper sheet is added into a copper sheet, a copper sheet is uniformly stirred, a copper sheet is prepared by a sodium hydroxide slurry, a copper sheet added into a copper sheet, a silicon substrate, a copper sheet is stirred, a copper sheet is stirred uniformly stirred, a copper sheet is added into a copper sheet, a copper.
The invention utilizes copper ions 1+ and 2+ to increase gap filling defects for replacing zinc elements, and utilizes an X-ray diffractometer to analyze that the invention forms blue-violet double peaks at 425nm and 445 nm.
The above-mentioned embodiments are only for convenience of description, and are not intended to limit the present invention in any way, and those skilled in the art will understand that the technical features of the present invention can be modified or changed by other equivalent embodiments without departing from the scope of the present invention.
Claims (4)
1, nanometer zinc oxide with indium element adulterant, which is characterized in that the nanometer zinc oxide comprises more than 99 wt% of zinc part, th indium element adulterant part and second cobalt element and copper element adulterant part;
the indium dopant moiety and the second cobalt and copper dopant moiety are present in a 1:1.5 weight ratio;
the indium element adulterant part, the second cobalt element adulterant part and the copper element adulterant part are doped into the zinc oxide by adopting a radio frequency reactive sputtering method, wherein the sputtering conditions are that the pre-vacuum before sputtering is 5-6 Pa, the substrate is a silicon single crystal, the diameter of the sputtering target is 10mm, the purity of the sputtering target is more than 99.99 percent, the sputtering reaction gas is the mixed gas of argon and oxygen, the distance between the substrate and the metal zinc target is 50mm, the substrate temperature is 100 ℃ and 300 ℃, the sputtering power is 60-200W, the sputtering pressure is 1-3.8 Pa, and the sputtering time is 1-2 h;
mixing zinc oxide prepared by a sputtering method with water to prepare a nano zinc oxide aqueous suspension with the mass concentration of 5.8%, ultrasonically dispersing for 4-6 minutes, adding aluminum potassium sulfate with the mass of 1.8% of that of the nano zinc oxide, adding the mixture into a high-speed stirrer, stirring for 1 hour at the rotating speed of 3200r/min, dripping a sodium hydroxide solution within 2-3 minutes, transferring the mixture into a reaction kettle lined with polytetrafluoroethylene, placing the reaction kettle into a homogeneous reactor, and reacting at the temperature of 100-120 ℃ for 6-8 hours; and after the reaction is finished, cooling to room temperature, performing centrifugal separation, washing and drying to obtain the indium-doped nano zinc oxide.
2. The kinds of nanometer zinc oxide with indium element adulterant according to claim 1, wherein the metal zinc targets are provided with three groups, indium sheets, copper sheets and cobalt sheets are respectively and evenly placed on the three groups of metal zinc targets, the three groups of metal zinc targets are evenly arranged around the silicon single crystal substrate, the indium sheets account for 3% of the metal zinc targets, the copper sheets account for 1.1-2.5% of the metal zinc targets, and the cobalt sheets account for 1% of the metal zinc targets.
3. The kinds of nanometer zinc oxide doped with in element as claimed in claim 1, wherein the surface of the silicon single crystal substrate is plasma cleaned and passivated.
4. The nanometer zinc oxides with indium element adulterants in claim 1, wherein the silicon carbide is added to control the concentration of the adulterants in the annealing process of preparing the nanometer zinc oxides with indium element adulterants by the sputtering method of radio frequency reaction.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910912650.6A CN110735109A (en) | 2019-09-25 | 2019-09-25 | nanometer zinc oxide with indium element adulterant |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101403099A (en) * | 2008-10-06 | 2009-04-08 | 上海工程技术大学 | Method of manufacturing metal doping ZnO film |
| CN104416160A (en) * | 2013-09-11 | 2015-03-18 | 安泰科技股份有限公司 | High-density zinc oxide based target and preparation method thereof |
| CN107265494A (en) * | 2017-06-06 | 2017-10-20 | 安徽锦华氧化锌有限公司 | A kind of modified nano zinc oxide |
-
2019
- 2019-09-25 CN CN201910912650.6A patent/CN110735109A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101403099A (en) * | 2008-10-06 | 2009-04-08 | 上海工程技术大学 | Method of manufacturing metal doping ZnO film |
| CN104416160A (en) * | 2013-09-11 | 2015-03-18 | 安泰科技股份有限公司 | High-density zinc oxide based target and preparation method thereof |
| CN107265494A (en) * | 2017-06-06 | 2017-10-20 | 安徽锦华氧化锌有限公司 | A kind of modified nano zinc oxide |
Non-Patent Citations (1)
| Title |
|---|
| 李爱侠等: "Co, Cu共掺杂ZnO薄膜的结构及发光特性", 《发光学报》 * |
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