CN106939405A - A kind of preparation method of graphene/oxide complex optical film - Google Patents
A kind of preparation method of graphene/oxide complex optical film Download PDFInfo
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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
- C23C14/3485—Sputtering using pulsed power to the 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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/02—Pretreatment of the material to be coated
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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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/20—Carburising
Abstract
The invention discloses a kind of preparation method of graphene/oxide complex optical film.It is a kind of preparation for realizing graphene/oxide complex optical film by two-step method using double-deck glow plasma physics sputter-deposition technology on quartz plate.Specifically quartz plate acetone is cleaned, high pressure nitrogen drying and processing；High-purity low melting point and refractory metal target are cleaned as the metallic element sputtering source of oxide with acetone, while being passed through the synthesis atmospheric condition of a certain proportion of argon gas and oxygen as metal oxide；The substrate pre-processed and target sample are put into double-deck glow plasma sputtering chamber, the preparation of sull is realized using two-step process.
Description
Technical field
The present invention relates to a kind of preparation method of film, specially a kind of system of graphene/oxide complex optical film
Preparation Method, belongs to field of film preparation.
Background technology
Graphene is by sp2Hydbridized carbon atoms are constituted, and possess excellent optics, electricity and mechanical property, itself and semiconductor
Oxide material is combined, and can often give play to outstanding effect.As there are some researches show：Graphene and inorganic oxide
Nanocomposites, by quickly guiding light induced electron avoid that the photoelectricity of semiconductor particle can be greatly improved with hole-recombination
Performance.For example, zinc oxide is a kind of broad stopband direct band gap compound semiconductor materials, with excellent optically and electrically performance
Zinc oxide is allowd to launch blue light or black light, high resistance and high c-axis（002）The zinc-oxide film of preferred orientation is determined
It possesses good piezoelectric constant and electromechanical coupling factor, can be as piezoelectricity, acoustic-electric, acousto-optical device, zinc oxide films in addition
Film is also used as extraordinary solar cell window material, and it is relative to SnO2Film（FTO）、In2O3Film (ITO) has
There is the advantage that nontoxic, cheap, stability is high, easily etch, therefore, zinc oxide and the compound of graphene will be in photoelectric fields
With potential application value.
The preparation method of current existing graphene/oxide complex optical film has chemical deposition, sol-gel
Deng, but above-mentioned preparation method high cost, complex operation, the problems such as residue is more.
The content of the invention
The present invention asking in terms of the quick preparation such as high-quality, large area for graphene/oxide complex optical film
Topic, proposes to complete to penetrate into graphene composite film on sull surface with plasma physics sputtering sedimentation two-step method so that
The process controllability is good, quick, quality is high, low cost, is especially suitable for large area and prepares.
Realize the technical scheme is that：
The present invention provides a kind of preparation method of graphene/oxide complex optical film, be one kind on quartz plate using double
Layer glow plasma sputter deposition technology realizes the preparation of graphene/oxide complex optical film by two-step method.Tool
Body is to clean quartz plate acetone, high pressure nitrogen drying and processing；High-purity low melting point and refractory metal target as oxide gold
Belong to element sputtering source, cleaned with acetone, while being passed through the synthesis of a certain proportion of argon gas and oxygen as metal oxide
Atmospheric condition；The substrate pre-processed and target sample are put into double-deck glow plasma sputtering chamber, using following two step
Method technique realizes the preparation of sull：
Step one：The preparation of sull
（1）The pretreatment of target and matrix：Metallic element sputtering source using high pure metal as oxide, to itself and matrix quartz
Piece is pre-processed with acetone, then uses high pressure nitrogen drying and processing；The distance between matrix and target frame are adjusted, 16- is maintained at
22mm；Three electrodes are drawn from substrate, target, and vacuum furnace cavity respectively, substrate and target are heated using the pulse power,
And matrix and target material surface are respectively formed a floor plasma glow discharge area in coating process, by two layers of plasma glow discharge area
The film forming efficiency of overlapping enhancing metal；
（2）The preparation of metal oxide film：Argon gas and oxygen are filled with to body of heater so that air pressure reaches 5-30 Pa in body of heater, by base
Bulk voltage pressure regulation is to 200-300 V so that matrix carries out preheating in 5-10 minute and bombardment；Then regulation matrix voltage is 300-
500 V, target voltage-regulation to 900-1000V, control matrix electric current is in 1.0-2.5A, and source current is in 0.5-2.0A, plated film
Time is according to required thickness control in 10-30min；
Step 2：The preparation of graphene/oxide laminated film
（1）The pretreatment of target and matrix：The sull sample obtained in step one is placed on substrate of substrate stage as matrix,
Using high-purity redox graphene paper as target, it is placed on the target frame in sputtering chamber, between regulation substrate of substrate stage and target frame
Distance, be maintained at 18-22 mm；The preparation process of above-mentioned metal oxide film is repeated, by two layers of plasma glow discharge area
Overlapping enhancing film forming efficiency；
（2）The preparation of graphene/oxide laminated film：Argon gas is filled with to body of heater so that air pressure reaches 30-35Pa in body of heater,
By substrate cathode voltage pressure regulation to 200-300 V so that matrix carries out preheating in 5-10 minutes and bombarded；Then adjust matrix voltage
For 300-500 V, graphene target voltage-regulation to 750-850V, control substrate cathode electric current is in 1.8-2.2A, source current
In 0.8-1.2A, after insulation 10-30min plated films after aura and parameter stability.
The volume ratio of argon gas and oxygen is 5 in step one:1-10:1.
High pure metal is single or polynary subgroup element metal in step one.It is preferred that high pure metal is zinc, titanium, one kind of molybdenum
Or it is a variety of.Further preferred high pure metal is zinc.
Beneficial effect：
The characteristics of the inventive method and advantage are as follows：
（1）The present invention is using high pure metal element and graphene paper as target, in order to which the supply and supply that improve element reaction are imitated
Rate, forms double-deck glow plasma discharge around substrate and target, and film forming only needs 10-30min..
（2）The present invention forms the composite transparent membrane electrode of large-area high-quality by the sputtering reaction of element, film
Thickness is at 5-10 microns.
（3）The film surface quality that the present invention is obtained is high, and zinc oxide composition has the c-axis of height（002）Orientation, visible
Optical band mean transmissivity can reach more than 65%, and film can effectively shield ultraviolet light.
Brief description of the drawings
Fig. 1 is the X ray diffracting spectrum of graphene/zinc oxide composite film prepared by the present invention.Can be with by XRD spectrum
Find out that the laminated film zinc oxide composition of the invention being made has the c-axis of height（002）Orientation, halfwidth（FWHM）For
0.236 °, crystalline quality is good；Obvious graphene feature bulge can be observed between 0-30 °.
Fig. 2 is graphene/zinc oxide composite film surface atom force microscope picture prepared by the present invention.Film is averaged
Surface roughness Ra：5.9nm, it is very small, illustrate that film shows more smooth.By microphoto it can be seen that film surface is equal
It is even, there is regular columnar structure, illustrate that the preparation-obtained laminated film of the inventive method is uniform and well-formed.
Fig. 3 is the ultraviolet-visible spectrum of graphene/zinc oxide composite film prepared by the present invention, wherein (a) is purple
The light transmittance and (b) of outside-visible ray are absorption spectrum.Pass through light transmission rate and absorptivity of the ultraviolet-visible luminosity meter to film
Characterized, it can be deduced that, the laminated film prepared by the inventive method visible light wave range transmitance reach 65% with
On, and there is more strong absorption to the light of ultraviolet band.
Embodiment
Embodiment 1：
The present invention is that one kind realizes stone using double-deck glow plasma physics sputter-deposition technology on quartz plate by two-step method
The preparation of black alkene/zinc oxide complex optical film.The preparation of zinc-oxide film is realized using following two-step process.
Step one：The preparation of zinc-oxide film
（1）The pretreatment of target and matrix：With high purity zinc（99.99%）As the metallic element sputtering source of zinc oxide, to itself and base
Body quartz plate is pre-processed with acetone, then uses high pressure nitrogen drying and processing；The distance between matrix and target frame are adjusted, is kept
In 22mm；Three electrodes are drawn from substrate, target, and vacuum furnace cavity respectively, substrate and target are added using the pulse power
Heat, and matrix and target material surface are respectively formed a floor plasma glow discharge area in coating process, are put by two layers of plasma glow
The film forming efficiency of the overlapping enhancing metal in electric area.
（2）The preparation of metal zinc oxide film：7 are filled with to body of heater:1 argon gas and oxygen so that air pressure reaches 5 in body of heater
Pa, by matrix voltage pressure regulation to 250 V so that matrix carries out preheating in 5 minutes and bombarded；Then regulation matrix voltage is 350 V,
Target voltage-regulation is to 900V, and control matrix electric current is in 1.0A, and source current is in 0.5A, plated film time thickness control required for
System is in 10min；
Step 2：The preparation of graphene/zinc oxide composite film
（1）The pretreatment of target and matrix：The zinc oxide films membrane sample obtained in step one is placed on substrate of substrate stage as matrix,
With high-purity redox graphene paper（99.999%）As target, it is placed on the target frame in sputtering chamber, regulation substrate of substrate stage and target
The distance between material frame, is maintained at 18 mm；Above-mentioned film forming procedure is repeated, by the overlapping enhancing in two layers of plasma glow discharge area
Film forming efficiency.
（2）The preparation of graphene/zinc oxide composite film：A certain amount of argon gas is filled with to body of heater so that air pressure in body of heater
35Pa is reached, by substrate cathode voltage pressure regulation to 300 V so that matrix carries out preheating in 5 minutes and bombarded；Then regulation matrix is electric
Press as 350 V, graphene target voltage-regulation to 850V, control substrate cathode electric current in 2A, source current in 1A, treat aura and
10min plated films are incubated after parameter stability.
Embodiment 2：
The present invention is that one kind realizes stone using double-deck glow plasma physics sputter-deposition technology on quartz plate by two-step method
The preparation of black alkene/titanium oxide complex optical film.The preparation of zinc-oxide film is realized using following two-step process.
Step one：The preparation of thin film of titanium oxide
（1）The pretreatment of target and matrix：With high purity titanium（99.99%）As the metallic element sputtering source of titanium oxide, to itself and base
Body quartz plate（25 mm×25mm）Pre-processed with acetone, then used high pressure nitrogen drying and processing；Adjust matrix and target frame it
Between distance, be maintained at 18 mm；Three electrodes are drawn from substrate, target, and vacuum furnace cavity respectively, substrate and target are equal
Heated using the pulse power, and matrix and target material surface are respectively formed a floor plasma glow discharge area in coating process, by two
The film forming efficiency of the overlapping enhancing metal in floor plasma glow discharge area.
（2）The preparation of metal oxidation titanium film：5 are filled with to body of heater:1 argon gas and oxygen so that air pressure reaches 25 in body of heater
Pa, by matrix voltage pressure regulation to 300 V so that matrix carries out preheating in 10 minutes and bombarded；Then regulation matrix voltage is 450
V, then opens target voltage-regulation to 950V, control matrix electric current is in 2.0A, and source current is in 2.0A, and plated film time is according to institute
Thickness control is needed in 15 min；
Step 2：The preparation of graphene/titanium oxide composite film
（1）The pretreatment of target and matrix：The thin film of titanium oxide sample obtained in step one is placed on substrate of substrate stage as matrix,
With high-purity redox graphene paper（99.999%）As target, it is placed on the target frame in sputtering chamber, regulation substrate of substrate stage and target
The distance between material frame, is maintained at 18 mm；Above-mentioned film forming procedure is repeated, by the overlapping enhancing in two layers of plasma glow discharge area
Film forming efficiency.
（2）The preparation of graphene/titanium oxide composite film：30Pa argon gas is filled with to body of heater, by substrate cathode voltage pressure regulation
To 300 V so that matrix carries out preheating in 5 minutes and bombarded；Then regulation matrix voltage is 350 V, and graphene target voltage is adjusted
Section to 850V, control substrate cathode electric current is plated in 2.2A, source current in 1.5A after being incubated 20min after aura and parameter stability
Film.
Embodiment 3：
The present invention is that one kind realizes stone using double-deck glow plasma physics sputter-deposition technology on quartz plate by two-step method
The preparation of black alkene/zinc oxide complex optical film.The preparation of zinc-oxide film is realized using following two-step process.
Step one：The preparation of zinc-oxide film
（1）The pretreatment of target and matrix：With high purity zinc（99.99%）As the metallic element sputtering source of zinc oxide, to itself and base
Body quartz plate is pre-processed with acetone, then uses high pressure nitrogen drying and processing；The distance between matrix and target frame are adjusted, is kept
In 16mm；Three electrodes are drawn from substrate, target, and vacuum furnace cavity respectively, substrate and target are added using the pulse power
Heat, and matrix and target material surface are respectively formed a floor plasma glow discharge area in coating process, are put by two layers of plasma glow
The film forming efficiency of the overlapping enhancing metal in electric area.
（2）The preparation of metal zinc oxide film：7 are filled with to body of heater:1 argon gas and oxygen so that air pressure reaches 5 in body of heater
Pa, by matrix voltage pressure regulation to 200 V so that matrix carries out preheating in 5 minutes and bombarded；Then regulation matrix voltage is 300 V,
Target voltage-regulation is to 900V, and control matrix electric current is in 1.0A, and source current is in 0.5A, plated film time thickness control required for
System is in 30min；
Step 2：The preparation of graphene/zinc oxide composite film
（1）The pretreatment of target and matrix：The zinc oxide films membrane sample obtained in step one is placed on substrate of substrate stage as matrix,
With high-purity redox graphene paper（99.999%）As target, it is placed on the target frame in sputtering chamber, regulation substrate of substrate stage and target
The distance between material frame, is maintained at 18 mm；Above-mentioned film forming procedure is repeated, by the overlapping enhancing in two layers of plasma glow discharge area
Film forming efficiency.
（2）The preparation of graphene/zinc oxide composite film：A certain amount of argon gas is filled with to body of heater so that air pressure in body of heater
30Pa is reached, by substrate cathode voltage pressure regulation to 300 V so that matrix carries out preheating in 5 minutes and bombarded；Then regulation matrix is electric
Press as 300 V, graphene target voltage-regulation to 850V, control substrate cathode electric current is in 1.8A, and source current treats brightness in 0.8A
30min plated films are incubated after light and parameter stability.
Claims (5)
1. a kind of preparation method of graphene/oxide complex optical film, it is characterised in that comprise the following steps：
Step one：The preparation of sull
（1）The pretreatment of target and matrix：Metallic element sputtering source using high pure metal as oxide, to itself and matrix quartz
Piece is pre-processed with acetone, then uses high pressure nitrogen drying and processing；The distance between matrix and target frame are adjusted, 16- is maintained at
22mm；Three electrodes are drawn from substrate, target, and vacuum furnace cavity respectively, substrate and target are heated using the pulse power,
And matrix and target material surface are respectively formed a floor plasma glow discharge area in coating process, by two layers of plasma glow discharge area
The film forming efficiency of overlapping enhancing metal；
（2）The preparation of metal oxide film：Argon gas and oxygen are filled with to body of heater so that air pressure reaches 5-30 Pa in body of heater, by base
Bulk voltage pressure regulation is to 200-300 V so that matrix carries out preheating in 5-10 minute and bombardment；Then regulation matrix voltage is 300-
500 V, target voltage-regulation to 900-1000V, control matrix electric current is in 1.0-2.5A, and source current is in 0.5-2.0A, plated film
Time is according to required thickness control in 10-30min；
Step 2：The preparation of graphene/oxide laminated film
（1）The pretreatment of target and matrix：The sull sample obtained in step one is placed on substrate of substrate stage as matrix,
Using high-purity redox graphene paper as target, it is placed on the target frame in sputtering chamber, between regulation substrate of substrate stage and target frame
Distance, be maintained at 18-22 mm；The preparation process of above-mentioned metal oxide film is repeated, by two layers of plasma glow discharge area
Overlapping enhancing film forming efficiency；
（2）The preparation of graphene/oxide laminated film：Argon gas is filled with to body of heater so that air pressure reaches 30-35Pa in body of heater,
By substrate cathode voltage pressure regulation to 200-300 V so that matrix carries out preheating in 5-10 minutes and bombarded；Then adjust matrix voltage
For 300-500 V, graphene target voltage-regulation to 750-850V, control substrate cathode electric current is in 1.8-2.2A, source current
In 0.8-1.2A, after insulation 10-30min plated films after aura and parameter stability.
2. preparation method according to claim 1, it is characterised in that the volume ratio of argon gas and oxygen is 5 in step one:
1-10:1。
3. preparation method according to claim 1, it is characterised in that high pure metal is single or polynary pair in step one
Race's metal element.
4. preparation method according to claim 3, it is characterised in that high pure metal is zinc, titanium, one kind of molybdenum or many
Kind.
5. preparation method according to claim 4, it is characterised in that high pure metal is zinc.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109267010A (en) * | 2018-11-29 | 2019-01-25 | 南京信息工程大学 | A kind of titanium oxygen compound flexible optoelectronic corrosion film and preparation method thereof |
| CN114351094A (en) * | 2021-12-20 | 2022-04-15 | 唐山万士和电子有限公司 | Production method of micro-balance quartz wafer with plating-enhanced graphite layer |
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| CN103147051A (en) * | 2013-03-08 | 2013-06-12 | 南京航空航天大学 | Preparation method of graphene iridium nanometer conductive catalytic film |
| CN103741094A (en) * | 2014-01-22 | 2014-04-23 | 武汉理工大学 | Preparation method of graphene composite conductive oxide target and transparent conductive film thereof |
| CN104319378A (en) * | 2014-10-09 | 2015-01-28 | 西安中科新能源科技有限公司 | Preparation method and application of oxide-coated tin alloy/graphene nano composite material |
| CN104393258A (en) * | 2014-10-09 | 2015-03-04 | 西安中科新能源科技有限公司 | Preparation method and use of oxide-coated silicon-titanium alloy/graphene nanometer composite material |
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2017
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| CN103147051A (en) * | 2013-03-08 | 2013-06-12 | 南京航空航天大学 | Preparation method of graphene iridium nanometer conductive catalytic film |
| CN103741094A (en) * | 2014-01-22 | 2014-04-23 | 武汉理工大学 | Preparation method of graphene composite conductive oxide target and transparent conductive film thereof |
| CN104319378A (en) * | 2014-10-09 | 2015-01-28 | 西安中科新能源科技有限公司 | Preparation method and application of oxide-coated tin alloy/graphene nano composite material |
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| CN109267010A (en) * | 2018-11-29 | 2019-01-25 | 南京信息工程大学 | A kind of titanium oxygen compound flexible optoelectronic corrosion film and preparation method thereof |
| CN114351094A (en) * | 2021-12-20 | 2022-04-15 | 唐山万士和电子有限公司 | Production method of micro-balance quartz wafer with plating-enhanced graphite layer |
| CN114351094B (en) * | 2021-12-20 | 2023-08-04 | 唐山万士和电子有限公司 | Production method of plating graphite layer microbalance quartz wafer |
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