CN106939405B - 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 methods 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；The metallic element sputtering source of high-purity low melting point and refractory metal target as oxide, is cleaned 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 technique
Graphene is by sp2Hydbridized carbon atoms are constituted, and have excellent optics, electricity and mechanical property, with semiconductor
Oxide material is compound, can often play outstanding effect.As existing research shows: graphene and inorganic oxide
Nanocomposites avoid the photoelectricity that semiconductor particle can be greatly improved with hole-recombination by quickly guiding light induced electron
Performance.For example, zinc oxide is a kind of broad stopband direct band gap compound semiconductor materials, there is excellent optically and electrically performance
Zinc oxide is allowed to emit blue light or black light, the zinc-oxide film decision of high resistance and high c-axis (002) preferred orientation
It has good piezoelectric constant and electromechanical coupling factor, can be used as piezoelectricity, acoustic-electric, acousto-optical device, furthermore zinc oxide films
Film is also used as extraordinary solar battery window material, relative to SnO2Film (FTO), In2O3Film (ITO) tool
There is the advantage that nontoxic, cheap, stability is high, is easy etching, therefore, zinc oxide and the compound of graphene will be in photoelectric fields
It has potential application.
The preparation method of current existing graphene/oxide complex optical film has chemical deposition, sol-gel
Deng the problems such as but above-mentioned preparation method is at high cost, complicated for operation, and residue is more.
Summary of the invention
The present invention asking in terms of high quality, large area etc. quickly preparation 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, at low cost, is especially suitable for large area preparation.
Realize the technical scheme is that
The present invention provides a kind of preparation method of graphene/oxide complex optical film, is that one kind is sharp on quartz plate
The system of graphene/oxide complex optical film is realized by two-step method with double-deck glow plasma physics sputter-deposition technology
It is standby.Specifically quartz plate acetone is cleaned, high pressure nitrogen drying and processing；High-purity low melting point and refractory metal target are as oxide
Metallic element sputtering source, cleaned with acetone, while being passed through a certain proportion of argon gas and oxygen as metal oxide
Synthesize atmospheric condition；The substrate pre-processed and target sample are put into double-deck glow plasma sputtering chamber, using as follows
The preparation of two-step process realization sull:
Step 1: the preparation of sull
(1) pretreatment of target and matrix: the metallic element sputtering source using high pure metal as oxide, to itself and matrix
Quartz plate is pre-processed with acetone, then with high pressure nitrogen drying and processing；The distance between matrix and target frame are adjusted, is maintained at
16-22mm；Three electrodes are drawn from substrate, target and vacuum furnace cavity respectively, substrate and target are all made of the pulse power and add
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) preparation of metal oxide film: being filled with argon gas and oxygen to furnace body, so that air pressure reaches 5-30 Pa in furnace body,
By matrix voltage pressure regulation to 200-300 V, so that matrix carries out preheating in 5-10 minutes and bombardment；Then adjusting matrix voltage is
300-500 V, target voltage are adjusted to 900-1000V, control matrix electric current in 1.0-2.5A, source current 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) pretreatment of target and matrix: matrix is placed in using sull sample obtained in step 1 as matrix
On platform, using high-purity redox graphene paper as target, it is placed on the indoor target frame of sputtering, adjusts substrate of substrate stage and target frame
The distance between, it is maintained at 18-22 mm；The preparation process for repeating above-mentioned metal oxide film, puts by two layers of plasma glow
The overlapping enhancing film forming efficiency in electric area；
(2) preparation of graphene/oxide laminated film: being filled with argon gas to furnace body, so that air pressure reaches 30- in furnace body
35Pa, by substrate cathode voltage pressure regulation to 200-300 V, so that matrix carries out preheating in 5-10 minutes and bombardment；Then adjust base
Bulk voltage is 300-500 V, and graphene target voltage is adjusted to 750-850V, controls substrate cathode electric current in 1.8-2.2A, source
Electrode current keeps the temperature 10-30min plated film in 0.8-1.2A after aura and parameter stability.
The volume ratio of argon gas and oxygen is 5:1-10:1 in step 1.
High pure metal is single or polynary subgroup element metal in step 1.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.
The utility model has the advantages that
The characteristics of the method for the present invention and advantage are as follows:
(1) present invention is using high pure metal element and graphene paper as target, in order to improve the supply and confession of element reaction
Efficiency is answered, forms double-deck glow plasma discharge around substrate and target, film forming only needs 10-30min..
(2) 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 obtains is high, and there is zinc oxide composition the c-axis (002) of height to be orientated, visible
Optical band mean transmissivity can reach 65% or more, and film can effectively shield ultraviolet light.
Detailed description of the invention
Fig. 1 is graphene/zinc oxide composite film X ray diffracting spectrum prepared by the present invention.It can be with by XRD spectrum
Find out that there is the laminated film zinc oxide composition that the present invention is made the c-axis (002) of height to be orientated, halfwidth (FWHM) is
0.236 °, crystalline quality is good；Apparent 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 average
Surface roughness Ra: 5.9nm, it is very small, it is more smooth to illustrate that film shows.By microphoto it can be seen that film surface is equal
It is even, there is regular columnar structure, illustrate the preparation-obtained laminated film of the method for the present invention uniformly and well-formed.
Fig. 3 is graphene/zinc oxide composite film ultraviolet-visible spectrum prepared by the present invention, wherein (a) is purple
Outside-visible light light transmittance and (b) be absorption spectrum.By ultraviolet-visible luminosity meter to the light transmission rate and absorptivity of film
Characterized, it can be deduced that, the laminated film being prepared by the method for the present invention visible light wave range transmitance reach 65% with
On, and there is more strong absorption to the light of ultraviolet band.
Specific embodiment
Embodiment 1:
The present invention is that one kind passes through two-step method reality using double-deck glow plasma physics sputter-deposition technology on quartz plate
The preparation of existing graphene/zinc oxide complex optical film.The preparation of zinc-oxide film is realized using following two-step process.
Step 1: the preparation of zinc-oxide film
(1) pretreatment of target and matrix: using high purity zinc (99.99%) as the metallic element sputtering source of zinc oxide, to it
It is pre-processed with matrix quartz plate with acetone, then with high pressure nitrogen drying and processing；The distance between matrix and target frame are adjusted,
It is maintained at 22mm；Three electrodes are drawn from substrate, target and vacuum furnace cavity respectively, substrate and target are all made of pulse electricity
Source heating, and matrix and target material surface are respectively formed a floor plasma glow discharge area in coating process, by two layers of plasma brightness
The film forming efficiency of the overlapping enhancing metal of light region of discharge.
(2) preparation of metal zinc oxide film: the argon gas and oxygen of 7:1 are filled with to furnace body, so that air pressure reaches 5 in furnace body
Pa, by matrix voltage pressure regulation to 250 V, so that matrix carries out preheating in 5 minutes and bombardment；Then adjusting matrix voltage is 350 V,
Target voltage is adjusted to 900V, controls matrix electric current in 1.0A, source current is in 0.5A, and plated film time is according to required thickness control
System is in 10min；
Step 2: graphene/zinc oxide composite film preparation
(1) pretreatment of target and matrix: matrix is placed in using zinc oxide films membrane sample obtained in step 1 as matrix
On platform, using high-purity redox graphene paper (99.999%) as target, it is placed on the indoor target frame of sputtering, adjusts matrix
The distance between platform and target frame are maintained at 18 mm；Above-mentioned film forming procedure is repeated, is handed over by two layers of plasma glow discharge area
Folded enhancing film forming efficiency.
(2) graphene/zinc oxide composite film preparation: being filled with a certain amount of argon gas to furnace body, so that air pressure in furnace body
Reach 35Pa, by substrate cathode voltage pressure regulation to 300 V, so that matrix carries out preheating in 5 minutes and bombardment；Then adjust matrix electricity
Pressure is 350 V, and graphene target voltage is adjusted to 850V, control substrate cathode electric current in 2A, source current in 1A, to aura and
10min plated film is kept the temperature after parameter stability.
Embodiment 2:
The present invention is that one kind passes through two-step method reality using double-deck glow plasma physics sputter-deposition technology on quartz plate
The preparation of existing graphene/titanium oxide complex optical film.The preparation of zinc-oxide film is realized using following two-step process.
Step 1: the preparation of thin film of titanium oxide
(1) pretreatment of target and matrix: using high purity titanium (99.99%) as the metallic element sputtering source of titanium oxide, to it
It is pre-processed with matrix quartz plate (25 mm × 25mm) with acetone, then with high pressure nitrogen drying and processing；Adjust matrix and target
The distance between frame is maintained at 18 mm；Three electrodes, substrate and target are drawn from substrate, target and vacuum furnace cavity respectively
Material is all made of pulse power heating, and matrix and target material surface are respectively formed a floor plasma glow discharge area in coating process,
By the film forming efficiency of the overlapping enhancing metal in two layers of plasma glow discharge area.
(2) preparation of metal oxidation titanium film: the argon gas and oxygen of 5:1 are filled with to furnace body, so that air pressure reaches 25 in furnace body
Pa, by matrix voltage pressure regulation to 300 V, so that matrix carries out preheating in 10 minutes and bombardment；Then adjusting matrix voltage is 450
V then opens target voltage and is adjusted to 950V, controls matrix electric current in 2.0A, source current is in 2.0A, and plated film time is according to institute
Need thickness control in 15 min；
Step 2: graphene/titanium oxide composite film preparation
(1) pretreatment of target and matrix: matrix is placed in using thin film of titanium oxide sample obtained in step 1 as matrix
On platform, using high-purity redox graphene paper (99.999%) as target, it is placed on the indoor target frame of sputtering, adjusts matrix
The distance between platform and target frame are maintained at 18 mm；Above-mentioned film forming procedure is repeated, is handed over by two layers of plasma glow discharge area
Folded enhancing film forming efficiency.
(2) graphene/titanium oxide composite film preparation: being filled with 30Pa argon gas to furnace body, by substrate cathode voltage pressure regulation
To 300 V, so that matrix carries out preheating in 5 minutes and bombardment；Then adjusting matrix voltage is 350 V, graphene target voltage tune
Section controls substrate cathode electric current in 2.2A, source current keeps the temperature 20min plating in 1.5A after aura and parameter stability to 850V
Film.
Embodiment 3:
The present invention is that one kind passes through two-step method reality using double-deck glow plasma physics sputter-deposition technology on quartz plate
The preparation of existing graphene/zinc oxide complex optical film.The preparation of zinc-oxide film is realized using following two-step process.
Step 1: the preparation of zinc-oxide film
(1) pretreatment of target and matrix: using high purity zinc (99.99%) as the metallic element sputtering source of zinc oxide, to it
It is pre-processed with matrix quartz plate with acetone, then with high pressure nitrogen drying and processing；The distance between matrix and target frame are adjusted,
It is maintained at 16mm；Three electrodes are drawn from substrate, target and vacuum furnace cavity respectively, substrate and target are all made of pulse electricity
Source heating, and matrix and target material surface are respectively formed a floor plasma glow discharge area in coating process, by two layers of plasma brightness
The film forming efficiency of the overlapping enhancing metal of light region of discharge.
(2) preparation of metal zinc oxide film: the argon gas and oxygen of 7:1 are filled with to furnace body, so that air pressure reaches 5 in furnace body
Pa, by matrix voltage pressure regulation to 200 V, so that matrix carries out preheating in 5 minutes and bombardment；Then adjusting matrix voltage is 300 V,
Target voltage is adjusted to 900V, controls matrix electric current in 1.0A, source current is in 0.5A, and plated film time is according to required thickness control
System is in 30min；
Step 2: graphene/zinc oxide composite film preparation
(1) pretreatment of target and matrix: matrix is placed in using zinc oxide films membrane sample obtained in step 1 as matrix
On platform, using high-purity redox graphene paper (99.999%) as target, it is placed on the indoor target frame of sputtering, adjusts matrix
The distance between platform and target frame are maintained at 18 mm；Above-mentioned film forming procedure is repeated, is handed over by two layers of plasma glow discharge area
Folded enhancing film forming efficiency.
(2) graphene/zinc oxide composite film preparation: being filled with a certain amount of argon gas to furnace body, so that air pressure in furnace body
Reach 30Pa, by substrate cathode voltage pressure regulation to 300 V, so that matrix carries out preheating in 5 minutes and bombardment；Then adjust matrix electricity
Pressure is 300 V, and graphene target voltage is adjusted to 850V, controls substrate cathode electric current in 1.8A, source current is in 0.8A, to brightness
30min plated film is kept the temperature after light and parameter stability.
Claims (5)
1. a kind of preparation method of graphene/oxide complex optical film, it is characterised in that the following steps are included:
Step 1: the preparation of sull
(1) pretreatment of target and matrix: the metallic element sputtering source using metal as oxide, to itself and matrix quartz plate use
Acetone is pre-processed, then with high pressure nitrogen drying and processing；The distance between matrix and target frame are adjusted, 16-22mm is maintained at；
Three electrodes are drawn from substrate, target and vacuum furnace cavity respectively, substrate and target are all made of the pulse power and heat, and
Matrix and target material surface are respectively formed a floor plasma glow discharge area in coating process, are overlapped by two layers of plasma glow discharge area
Enhance the film forming efficiency of metal；
(2) preparation of metal oxide film: being filled with argon gas and oxygen to furnace body, so that air pressure reaches 5-30 Pa in furnace body, by base
Bulk voltage pressure regulation is to 200-300 V, so that matrix carries out preheating in 5-10 minutes and bombardment；Then adjusting matrix voltage is 300-
500 V, target voltage are adjusted to 900-1000V, control matrix electric current in 1.0-2.5A, 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) pretreatment of target and matrix: being placed on substrate of substrate stage using sull sample obtained in step 1 as matrix,
Using redox graphene paper as target, be placed on the indoor target frame of sputtering, adjust between substrate of substrate stage and target frame away from
From being maintained at 18-22 mm；The preparation process for repeating above-mentioned metal oxide film, it is overlapping by two layers of plasma glow discharge area
Enhance film forming efficiency；
(2) preparation of graphene/oxide laminated film: being filled with argon gas to furnace body, so that air pressure reaches 30-35Pa in furnace body,
By substrate cathode voltage pressure regulation to 200-300 V, so that matrix carries out preheating in 5-10 minutes and bombardment；Then adjust matrix voltage
For 300-500 V, graphene target voltage is adjusted to 750-850V, controls substrate cathode electric current in 1.8-2.2A, source current
In 0.8-1.2A, 10-30min plated film is kept the temperature after aura and parameter stability.
2. preparation method according to claim 1, which is characterized in that the volume ratio of argon gas and oxygen is 5 in step 1:
1-10:1。
3. preparation method according to claim 1, which is characterized in that metal described in step 1 is single or polynary pair
Race's metal element.
4. preparation method according to claim 3, which is characterized in that the metal is zinc, titanium, one kind of molybdenum or more
Kind.
5. preparation method according to claim 4, which is characterized in that the metal is zinc.
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Effective date of registration: 20221209 Address after: No. 38, Fenghuangshan Road, Science and Technology Industrial Park, Dongshan Town, Wuzhong District, Suzhou City, Jiangsu Province, 215000 Patentee after: WOOJIN ACT (SUZHOU) CO.,LTD. Address before: 210044, No. 219, Ning six road, Pukou District, Jiangsu, Nanjing Patentee before: Nanjing University of Information Science and Technology |