CN108914077A - One kind being based on Nb2O5Transparent conductive oxide film and preparation method thereof - Google Patents
One kind being based on Nb2O5Transparent conductive oxide film and preparation method thereof Download PDFInfo
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- CN108914077A CN108914077A CN201810870166.7A CN201810870166A CN108914077A CN 108914077 A CN108914077 A CN 108914077A CN 201810870166 A CN201810870166 A CN 201810870166A CN 108914077 A CN108914077 A CN 108914077A
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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
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron 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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/083—Oxides of refractory metals or yttrium
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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
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
Abstract
The invention discloses one kind to be based on Nb2O5Transparent conductive oxide film and preparation method thereof, the film is made of substrate, bottom Metal Oxide film layer, intermediate metal layer and top metal oxide film layer, wherein, substrate is glass, and bottom Metal Oxide film layer is the Nb deposited using radio frequency magnetron sputtering method2O5Layer, intermediate metal layer is the Ag layer deposited using the method for magnetically controlled DC sputtering, top metal oxide film layer is the ZnO layer deposited using radio frequency magnetron sputtering method, the thickness of bottom Metal Oxide film layer and top metal oxide film layer is 35~55nm, intermediate metal layer with a thickness of 8~20nm.The film is not only cheap, asepsis environment-protecting, but also is to prepare at room temperature, without heating, simplifies preparation process, has the possibility for replacing traditional ITO to be widely used in optoelectronic materials technology.
Description
Technical field
The invention belongs to optoelectronic materials technologies, and in particular to a kind of to be efficiently based on Nb2O5Transparent conductive oxide
Film and preparation method thereof.
Background technique
Transparent conductive oxide film is a kind of important photoelectric material, because its have close to metal electric conductivity, compared with
The high transparency and the characteristics such as the high reflectance of infrared ray are widely used in solar battery, flat-panel monitor and thoroughly
In the preparation such as photopic vision window, become indispensable a kind of film.
There are two types of conduction type, i.e. N-shaped and p-type, N-shaped transparent conductive oxide film electricity for transparent conductive oxide film tool
Resistance rate is up to 10-3~10-5Ω cm is got a lot of applications in fields such as photoelectric device, solar batteries；P-type electrically conducting transparent oxygen
The production p-n junction that is prepared as of compound film is laid a good foundation, and has expanded transparent conductive film broader practice prospect.
In the preparation of transparent conductive film, common physical method have vacuum evaporation coating membrane technology, sputter coating technology,
Ion beam assisted depositing coating technique, pulsed laser deposition technique etc.；Wherein, sputter coating is to use ion bombardment target material surface,
It is shelled out the atom of target, the atom of sputtering is then deposited on a kind of coating technique that long-pending body surface face forms film, this kind
Oneself of the film thickness controllability of technology and strong, the easy realization large area of the binding ability of reproducible, applied widely, film and substrate
Dynamic metaplasia produces.Therefore it is widely used in field of photoelectric technology this method.Target preferable for electric conductivity, usually makes
With magnetically controlled DC sputtering technology, and for needing the nonmetallic target of very high voltage then mostly complete using radiofrequency magnetron sputtering technology
At plated film.
In the prior art, indium tin oxide (ITO) is that a kind of comprehensive photoelectric properties are excellent and in field of optoelectronic devices
Widely used transparent conductive oxide.But ITO preparation process is complex, indium metal belongs to scarce resource again, because
And the cost of manufacture of this kind of material is higher, and has certain toxicity, these conditions all make ITO in use by one
Fixed is restricted.
ZnO film is a kind of novel, multiduty semiconductor material with wide forbidden band, forbidden bandwidth 3.3eV.Its light transmission
Property be higher than 90%.Intrinsic ZnO crystal has the conductive characteristic of N-shaped, and carrier concentration and electron mobility are all very high, and natural
Rich reserves in boundary.Nb2O5It is a kind of semiconductor material that forbidden bandwidth is 3.6eV, in visible light and near-infrared optical wavelength model
It is with preferable optical transmittance.Its physical property and chemical property are more stable, in optical interference filter, solar-electricity
Many modern technologies fields such as pond have many applications.By the preparation of both material applications to transparent conductive oxide film
It is middle will be for preparation high-performance and cheap transparent conductive oxide film provides possibility.
Summary of the invention
In view of the above problems, the present invention is intended to provide providing a kind of based on Nb2O5Transparent conductive oxide it is thin
Film, the film is not only cheap, asepsis environment-protecting, but also is to prepare at room temperature, without heating, simplifies preparation process,
There is the possibility for replacing traditional ITO to be widely used in optoelectronic materials technology in future.
To achieve the goals above, the technical solution adopted in the present invention is as follows：One kind being based on Nb2O5Electrically conducting transparent oxygen
Compound film is made of substrate, bottom Metal Oxide film layer, intermediate metal layer and top metal oxide film layer,
In, substrate is glass, and bottom Metal Oxide film layer is the Nb deposited using radio frequency magnetron sputtering method2O5Layer, intermetallic metal
Layer is the Ag layer deposited using the method for magnetically controlled DC sputtering, and top metal oxide film layer is using rf magnetron sputtering side
The ZnO layer of method deposition.
Further, the thickness of the bottom Metal Oxide film layer and top metal oxide film layer be 35~
55nm, intermediate metal layer with a thickness of 8~20nm.
One kind being based on Nb2O5Transparent conductive oxide film preparation method, specific preparation step is：
1) processing of substrate；Glass substrate is successively cleaned by ultrasonic 15 in deionized water, acetone and ethanol solution respectively
~20min is put into sputtering chamber after being dried up after cleaning with high pure nitrogen；
2) pre-sputtering of target：The Nb for being 99.9% by purity2O5Target and ZnO target utilize radio frequency magnetron in sputtering chamber
The method of sputtering distinguishes 10~15min of pre-sputtering, and the Ag target that purity is 99.9% is being utilized direct magnetic control in sputtering chamber
Method 10~15min of pre-sputtering of sputtering, sputtering chamber background vacuum are evacuated to 6 × 10-4Pa, being filled with purity in sputtering process is
99.99% argon gas is as sputter gas；
3)Nb2O5The sputtering of layer：Nb is prepared using the method for rf magnetron sputtering on substrate2O5Layer, it is filled in sputtering process
Enter the argon gas that purity is 99.99% as sputter gas, operating pressure at room temperature is 1.0pa；
4) Ag layers of sputtering：In Nb2O5Ag layers are prepared using the method for magnetically controlled DC sputtering on layer, is filled in sputtering process
The argon gas that purity is 99.99% is as sputter gas；
5) sputtering of ZnO layer：ZnO layer is prepared using the method for rf magnetron sputtering on Ag layer, is filled in sputtering process
The argon gas that purity is 99.99% is as sputter gas.
Further, the radio-frequency power of the step 3) is 100W.
Further, the radio-frequency power of the step 4) is 20W.
Further, the radio-frequency power of the step 5) is 100W.
The beneficial effects of the invention are as follows：Compared with traditional oxide electroconductive film, Nb2O5/ Ag/ZnO high-efficient transparent is conductive
The material source range of sull is wider, and resourceful, cost of material is lower；The sheet resistance of different materials is smaller,
Light transmittance with higher in visible-range；It does not need to heat during preparation, can prepare under room temperature
Film with good photoelectric properties, preparation process are simple；In addition to this, it can be used as the electrode of organic electro-optic device, ZnO can be with
As electron transfer layer, so Nb2O5/ Ag/ZnO transparent conductive film can also do the middle layer of series-connected solar cells, application
Range is wide, practical.
Detailed description of the invention
Fig. 1 is of the invention a kind of based on Nb2O5Transparent conductive oxide film structural schematic diagram；
Fig. 2 is the Nb of method preparation disclosed by the invention2O5The translucency of/Ag/ZnO transparent conductive oxide film and ITO
Comparison diagram；
Fig. 3 is the Nb of method preparation disclosed by the invention2O5The electric conductivity of/Ag/ZnO transparent conductive oxide film and ITO
Comparison diagram.
Specific embodiment
In order to make those skilled in the art be better understood on technical solution of the present invention, with reference to the accompanying drawing and
Embodiment is further described technical solution of the present invention.
Embodiment one：One kind being based on Nb2O5Transparent conductive oxide film structure it is as shown in Fig. 1, the present invention preparation
Film be transparent multilaminar structure, the oxide of upper and lower level mainly have of both act on：(1) intermediate metal layer holds in air
It is easily oxidized, upper and lower level oxide can be effectively protected intermediate metal layer from being oxidized, to improve the steady of multilayered structure
It is qualitative；(2) although single metal material has preferable electric conductivity, compared with sull, translucency compares
Difference.The oxide of upper and lower level is the material of broad-band gap, and translucency with higher can effectively make up metal material translucency
The defect of difference, improves the translucency of entire multi-layered electrode.
Nb of the invention2O5In/Ag/ZnO electrically conducting transparent plural layers, the effect of intermediate metal layer Ag mainly determines whole
The electric conductivity of a structure, because oxide used in the present invention is all semiconductor material, conductivity is smaller.And intermetallic metal material
Material usually has very high conductivity, can effectively improve entire plural layers when metal material is clipped among oxide
Electric conductivity.
The specific preparation step of this kind of film is：
1. the processing of substrate：Substrate is 20mm × 20mm × 1mm glass, by substrate successively in deionization before sputtering
Water, acetone are cleaned by ultrasonic 15min in ethanol solution respectively, to remove the particle and organic pollutant of substrate surface, finally with height
Pure nitrogen gas drying is put into sputtering chamber；
2. sputtering chamber background vacuum is evacuated to 6 × 10-4Pa is filled with the argon gas of high-purity in sputtering process
(99.99%) it is used as sputter gas；
3. the pretreatment of target：Nb2O5Target purity is 99.9%, and ZnO target purity is that 99.9%, Ag target purity is 99.9%,
By Nb2O5Ag target is utilized magnetically controlled DC sputtering using the method difference pre-sputtering 10min of rf magnetron sputtering by target and ZnO target
Method pre-sputtering 10min, pre-sputtering is the impurity and pollutant in order to remove target material surface, to improve Nb2O5,ZnO and Ag film
Quality；
4.Nb2O5The sputtering of layer:Nb is prepared using the method for rf magnetron sputtering on substrate2O5Layer, sputtering process are filled with
The argon gas (99.99%) of high-purity is used as sputter gas, and operating pressure is 1.0Pa at room temperature, uses the radio-frequency power of 100W
Sputtering, with a thickness of 35~55nm；
5.Ag layers of sputtering：In Nb2O5Ag layers are prepared using the method for magnetically controlled DC sputtering on layer, sputtering process is filled with height
The argon gas of purity is sputtered, with a thickness of 8~20nm as sputter gas using the dc power of 20W.
The sputtering of 6.ZnO:ZnO layer is prepared using the method for rf magnetron sputtering on Ag layer, is filled in sputtering process pure
The argon gas that degree is 99.99% is as sputter gas, radio-frequency power 100W, with a thickness of 35~55nm.
Embodiment two：With the commercialization of the multi-layer transparent conductive oxide film prepared in embodiment one and laboratory purchase
ITO is the comparison that test material carries out specific nature.
Measuring device is as follows：
Translucency is to measure gained using ultraviolet-visible spectrophotometer (Lambda 35, PerkinElmer)；
Electric conductivity is to measure gained using four probes (ST-2258A).
Fig. 2 is Nb2O5The transmittance spectrum figure of/Ag/ZnO film and ITO, as can be seen from Figure 2 Nb2O5/ Ag/ZnO film
Translucency is better than ITO, and translucency reaches 90% or more in visible-range.
Fig. 3 is Nb2O5The electric conductivity comparison diagram of/Ag/ZnO film and ITO in six months, as can be seen from Figure 3 Nb2O5/
The stability of Ag/ZnO film and ITO are all very superior, but Nb2O5The sheet resistance of/Ag/ZnO film is only 4.8 Ω/sq, excellent
In ITO.
To sum up, Nb2O5/ Ag/ZnO film is not only cheap, asepsis environment-protecting, but also is to prepare at room temperature, without plus
Heat simplifies preparation process, and film prepared by the present invention is better than ITO in translucency, stability and sheet resistance, this is just
Illustrate that this thin-film material in the following potential for existing and traditional ITO being replaced to be widely used in optoelectronic materials technology, is
More extensive thinking has been opened up in the preparation of the transparent conductive film of field of photoelectric technology.
Basic principles and main features and advantage of the invention have been shown and described above.But the foregoing is merely this hairs
Bright specific embodiment, technical characteristic of the invention are not limited thereto, and any those skilled in the art is not departing from this hair
The other embodiments obtained under bright technical solution should all cover within the scope of the patent of the present invention.
Claims (6)
1. one kind is based on Nb2O5Transparent conductive oxide film, which is characterized in that the film is by substrate, bottom Metal Oxide
Film layer, intermediate metal layer and top metal oxide film layer composition, wherein substrate is glass, and bottom Metal Oxide is thin
Film layer is the Nb deposited using radio frequency magnetron sputtering method2O5Layer, intermediate metal layer is to be deposited using DC magnetron sputtering method
Ag layers, top metal oxide film layer is the ZnO layer deposited using radio frequency magnetron sputtering method.
2. as described in claim 1 a kind of based on Nb2O5Transparent conductive oxide film, which is characterized in that bottom gold
The thickness for belonging to oxide film layer and top metal oxide film layer is 35~55nm, intermediate metal layer with a thickness of 8~
20nm。
3. described in any item a kind of based on Nb as in claims 1 and 22O5Transparent conductive oxide film preparation method,
It is characterized in that, specific preparation step is：
1) processing of substrate；Glass substrate is successively cleaned by ultrasonic in deionized water, acetone and ethanol solution to 15 respectively~
20min is put into sputtering chamber after being dried up after cleaning with high pure nitrogen；
2) pre-sputtering of target：The Nb for being 99.9% by purity2O5Target and ZnO target utilize rf magnetron sputtering in sputtering chamber
Method distinguish 10~15min of pre-sputtering, by purity be 99.9% Ag target in sputtering chamber utilize magnetically controlled DC sputtering
Method 10~15min of pre-sputtering, sputtering chamber background vacuum is evacuated to 6 × 10-4Pa, being filled with purity in sputtering process is
99.99% argon gas is as sputter gas；
3)Nb2O5The sputtering of layer：Nb is prepared using the method for rf magnetron sputtering on substrate2O5Layer, it is filled in sputtering process pure
For the argon gas that degree is 99.99% as sputter gas, operating pressure at room temperature is 1.0pa；
4) Ag layers of sputtering：In Nb2O5Ag layers are prepared using the method for magnetically controlled DC sputtering on layer, purity is filled in sputtering process
For 99.99% argon gas as sputter gas；
5) sputtering of ZnO layer：ZnO layer is prepared using the method for rf magnetron sputtering on Ag layer, is filled with purity in sputtering process
For 99.99% argon gas as sputter gas.
4. as claimed in claim 3 a kind of based on Nb2O5Transparent conductive oxide film preparation method, which is characterized in that
The radio-frequency power of the step 3) is 100W.
5. as claimed in claim 3 a kind of based on Nb2O5Transparent conductive oxide film preparation method, which is characterized in that
The radio-frequency power of the step 4) is 20W.
6. as claimed in claim 3 a kind of based on Nb2O5Transparent conductive oxide film preparation method, which is characterized in that
The radio-frequency power of the step 5) is 100W.
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Cited By (4)
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| CN111769290A (en) * | 2020-08-11 | 2020-10-13 | 天津瑞晟晖能科技有限公司 | Application of nitrogen-doped niobium pentoxide in secondary battery, all-solid-state thin-film lithium ion battery, preparation method of all-solid-state thin-film lithium ion battery and electric equipment |
| CN112885503A (en) * | 2021-01-12 | 2021-06-01 | 南开大学 | Preparation method and application of ultrathin silver-based OMO (organic molybdenum oxide) composite transparent conductive film |
| CN113161043A (en) * | 2021-04-26 | 2021-07-23 | 中国科学院宁波材料技术与工程研究所 | Ultrathin metal transparent antenna and preparation method thereof |
| CN114231903A (en) * | 2021-12-08 | 2022-03-25 | 洛阳理工学院 | Niobium oxide/silver nanowire double-layer structure flexible transparent conductive film and preparation method thereof |
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Application publication date: 20181130 |