CN108950482A - A kind of ultraviolet 300nm is semi-transparent-copper and indium doped transparent conductive film and preparation method thereof - Google Patents

A kind of ultraviolet 300nm is semi-transparent-copper and indium doped transparent conductive film and preparation method thereof Download PDF

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CN108950482A
CN108950482A CN201810965660.1A CN201810965660A CN108950482A CN 108950482 A CN108950482 A CN 108950482A CN 201810965660 A CN201810965660 A CN 201810965660A CN 108950482 A CN108950482 A CN 108950482A
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conductive film
copper
ultraviolet
semi
preparation
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张治国
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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
    • 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
    • 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
    • C23C14/24—Vacuum evaporation
    • C23C14/26—Vacuum evaporation by resistance or inductive heating of the source
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The invention discloses a kind of ultraviolet 300nm it is semi-transparent-preparation method of copper and indium doped transparent conductive film, include the following steps: to take a circular mount disk, dig one 10 × 10cm therebetween2Square hole, be that a length of 100mm metal strip of 1mm is being fixed on the turntable of DM450A type coating machine in circular mount disk away from three holes are made a call at outer edge 5mm from a width is fastened at square hole edge 10.5mm；Two filaments are put on quartz boat to be fastened on heating electrode, by 12 × 12 clean × 0.15cm3Quartz glass be placed in above square hole, take 1000mg tin and 100mg copper, 100mg indium to be put into crucible, put down bell jar, open mechanical pump and carry out coating operation, after the completion, take out, be put into annealing furnace, anneal 25 minutes and take out at 450 DEG C.Conductive film of the invention is the semi-permeable membrane of a 300nm ultraviolet light, the light splitting for the ultraviolet instrumentation that can be used under this wavelength.

Description

A kind of ultraviolet 300nm is semi-transparent-copper and indium doped transparent conductive film and preparation method thereof
Technical field
The present invention relates to electronic component preparation fields, and in particular to and a kind of ultraviolet 300nm is semi-transparent-and copper and indium doping transparent is conductive Film and preparation method thereof.
Background technique
Transparent conductive film is a kind of widely used photoelectron material, such as solar battery, liquid crystal display device, electromagnetic wave Light transmission shielding, the electrode etc. of phosphor.It has high transparency, and high conductivity is corrosion-resistant to wait excellent properties.It is general Transparent conductive film hardly has transmitance in ultraviolet light spectral coverage, this for photovoltaic device application be it is unfavorable, because of the sun Big energy photon (such as ultraviolet light) in light can be fallen by this membrane filtration, to be unfavorable for the raising of photoelectric conversion efficiency.
Summary of the invention
To solve the above problems, the present invention provides a kind of ultraviolet 300nm it is semi-transparent-copper and indium doped transparent conductive film and its system Preparation Method.
To achieve the above object, the technical scheme adopted by the invention is as follows:
A kind of ultraviolet 300nm is semi-transparent-preparation method of copper and indium doped transparent conductive film, include the following steps:
S1,12 × 12 × 0.15cm is taken3Quartz glass, cleaned up in the sink with detergent, with cold and hot deionization Water rinses after five minutes, is put into spare in baking oven；
S2, the tungsten wire for being 0.8mm with diameter heat the circle of coiling filament 13 on the rod iron that diameter is 3mm, and both ends are respectively stayed 5cm, it is totally two, spare；
S3, the quartz ampoule for taking long 5cm diameter 1.5cm fire a pit in the middle and make load source crucible；
S4, a circular mount disk is taken, digs one 10 × 10cm therebetween2Square hole, then from square hole edge 10.5mm Place's one width of fastening is a length of 100mm metal strip of 1mm, in circular mount disk away from making a call to three holes, central angle every 120 at outer edge 5mm Degree one, is then screwed on the turntable of DM450A type coating machine；
S5, two filaments are put on quartz boat be fastened on heating electrode on, open power supply, press lower inverted bell liter button, to clock Clean quartz glass is placed in above the square hole of the circular mount disk when rising to the upper limit by cover, take 1000mg tin (Sn) and 100mg copper (Cu), 100mg indium (In) are put into silica crucible, put down bell jar, open mechanical pump, open diffusion pump after 20 points, and 30 High threshold is opened after minute, taking out bell jar vacuum degree is 3 × 10-3Pa is then turned on silicon power supply and maintains the temperature at 400 DEG C of left sides Needle-valve is unscrewed on the right side, is passed through high pure oxygen, and monitoring high vacuum meter gauge outfit is allowed to be maintained at 8.5-8.8 × 10-2Pa or so is opened Workpiece rotation controller and revolving speed is adjusted at 11 revs/min；Evaporation source current is opened, turn pressure regulator turntable makes heating power Baffle is opened after 165W or so, 1 minute, the growth rate control of film terminates after 10-12nm/min or so, 40 points, will add Thermoelectricity source power is reduced to 0, closes baffle, closes silicon power supply, closes substrate rotating disk power supply, closes oxygen, closes high Vacuum valve, after 15 minutes give bell jar inflation, after can't hear the hiss of inflation, take out plated film after glass, be put into annealing furnace, It anneals 25 minutes and takes out at 450 DEG C.
Further, when resulting conductive film 300nm transmitance be greater than 50% when, then should extend plated film time；When Resulting conductive film 300nm transmitance less than 50%, then should shorten plated film time or be appropriately extended annealing time.
The present invention also provides a kind of ultraviolet 300nm it is semi-transparent-copper and indium doped transparent conductive film, by above-mentioned preparation method system Standby gained.
The invention has the following advantages:
Conductive film of the invention is the semi-permeable membrane of a 300nm ultraviolet light, the ultraviolet instrumentation that can be used under this wavelength Light splitting.
Preparation process of the present invention is simple, using cheap Sn and Cu, it is only necessary to which prepared by the In of 100mg, at low cost.
Detailed description of the invention
Fig. 1 is the Transmissivity measurement result of each sample in the embodiment of the present invention.
Fig. 2 is the relationship of sample resistivity and temperature in the embodiment of the present invention.
Specific embodiment
In order to which objects and advantages of the present invention are more clearly understood, the present invention is carried out with reference to embodiments further It is described in detail.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to limit this hair It is bright.
Embodiment
A kind of ultraviolet 300nm is semi-transparent-preparation method of copper and indium doped transparent conductive film, include the following steps:
S1,12 × 12 × 0.15cm is taken3Quartz glass, 12 × 12 × 0.3cm3Corning7059 glass and same sample ruler Very little simple glass is cleaned up in the sink with detergent, is rinsed after five minutes, is put into standby in baking oven with cold and hot deionized water With；
S2, the tungsten wire for being 0.8mm with diameter heat the circle of coiling filament 13 on the rod iron that diameter is 3mm, and both ends are respectively stayed 5cm, it is totally two, spare；
S3, the quartz ampoule for taking long 5cm diameter 1.5cm fire a pit in the middle and make load source crucible；
S4, a circular mount disk is taken, digs one 10 × 10cm therebetween2Square hole, then from square hole edge 10.5mm Place's one width of fastening is a length of 100mm metal strip of 1mm, in circular mount disk away from making a call to three holes, central angle every 120 at outer edge 5mm Degree one, is then screwed on the turntable of DM450A type coating machine；
S5, two filaments are put on quartz boat be fastened on heating electrode on, open power supply, press lower inverted bell liter button, to clock Clean quartz glass is placed in above the square hole of the circular mount disk when rising to the upper limit by cover, take 1000mg tin (Sn) and 100mg copper (Cu), 100mg indium (In) are put into silica crucible, put down bell jar, open mechanical pump, open diffusion pump after 20 points, and 30 High threshold is opened after minute, taking out bell jar vacuum degree is 3 × 10-3Pa is then turned on silicon power supply and maintains the temperature at 400 DEG C of left sides Needle-valve is unscrewed on the right side, is passed through high pure oxygen, and monitoring high vacuum meter gauge outfit is allowed to be maintained at 8.5-8.8 × 10-2Pa or so is opened Workpiece rotation controller and revolving speed is adjusted at 11 revs/min；Evaporation source current is opened, turn pressure regulator turntable makes heating power Baffle is opened after 165W or so, 1 minute, the growth rate control of film terminates after 10-12nm/min or so, 40 points, will add Thermoelectricity source power is reduced to 0, closes baffle, closes silicon power supply, closes substrate rotating disk power supply, closes oxygen, closes high Vacuum valve, after 15 minutes give bell jar inflation, after can't hear the hiss of inflation, take out plated film after glass, be put into annealing furnace, It anneals 25 minutes and takes out at 450 DEG C, measure its square resistance, transmitance, film thickness, film thickness about 500nm or so.If film Deviate 50% in the transmitance of 300nm, then its transmitance of adjustable plastics thickness control.For example it can be appropriately extended greater than 50% Plated film time can shorten plated film time, or proper extension annealing time etc. if it is less than 50% and solve.
As seen from Figure 1, it should it is attracting great attention the result is that 5-5# film sample, at 900nm infrared light district Transmitance be about 95%, wavelength be 900nm~300nm in the range of, transmitance is slowly reduced with the reduction of wavelength, Transmitance at a length of 300nm of light wave is 52.5%, this is unique one sample for having high transmittance to ultraviolet light, simultaneously It is also a good semi-permeable membrane.The results show that using different substrates, its transmitance is slightly different, the 5#-8 in Fig. 1, 5#-9 is the measurement result of quartz glass substrate, and 5#-6 is the measurement result of corning7059 glass substrate, and 5#-5 is common glass The measurement result of glass substrate.Technology controlling and process error should be regarded as the transmitance difference of substrate of the same race.
Resistance-temperature characteristic is an important index, and after entering film for understanding copper atom, material is at a lower temperature Resistivity-temperature characteristic, the resistance-temperature characteristic for preparing film sample is tested, using two-probe method, is being reequiped HT-288 type high Tc superconducting material resistance afterwards-square resistance of temperature characteristic measuring instrument measurement sample and the relationship of temperature.Choosing Selecting temperature range is 77.4K~280K.See there is satisfied low resistance in wider temperature range by the measurement result of sample The case where rate, sees Fig. 2.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, without departing from the principle of the present invention, it can also make several improvements and retouch, these improvements and modifications are also answered It is considered as protection scope of the present invention.

Claims (4)

1. a kind of ultraviolet 300nm is semi-transparent-preparation method of copper and indium doped transparent conductive film, which comprises the steps of:
S1,12 × 12 × 0.15cm is taken3Quartz glass, cleaned up in the sink with detergent, with cold and hot deionized water rinse After five minutes, it is put into spare in baking oven；
S2, the tungsten wire for being 0.8mm with diameter heat the circle of coiling filament 13 on the rod iron that diameter is 3mm, and 5cm is respectively stayed at both ends, altogether It is two, spare；
S3, the quartz ampoule for taking long 5cm diameter 1.5cm fire a pit in the middle and make load source crucible；
S4, a circular mount disk is taken, digs one 10 × 10cm therebetween2Square hole, then from square hole edge 10.5mm fasten One width is a length of 100mm metal strip of 1mm, in circular mount disk away from making a call to three holes at outer edge 5mm, every 120 degree one, central angle, Then it is screwed on the turntable of DM450A type coating machine；
S5, two filaments are put on quartz boat be fastened on heating electrode on, open power supply, press lower inverted bell liter button, to bell jar liter Supreme to prescribe a time limit, four tenons clean quartz glass being placed in above the square hole of the circular mount disk take 1000mg tin It is put into silica crucible with 100mg copper, 100mg indium, puts down bell jar, opened mechanical pump, diffusion pump is opened after 20 points, after 30 minutes High threshold is opened, taking out bell jar vacuum degree is 3 × 10-3Pa is then turned on silicon power supply and maintains the temperature at 400 DEG C, unscrewing needle Valve, is passed through high pure oxygen, and monitoring high vacuum meter gauge outfit is allowed to be maintained at 8.5-8.8 × 10-2Pa opens workpiece rotation controller And revolving speed is adjusted at 11 revs/min；Evaporation source current is opened, turn pressure regulator turntable makes heating power after 165W, 1 minute Baffle is opened, the growth rate control of film terminates after 10-12nm/min, 40 points, heating power supply power is reduced to 0, closes gear Plate closes silicon power supply, closes substrate rotating disk power supply, closes oxygen, closes high vacuum valve, fills after 15 minutes to bell jar Gas, after can't hear the hiss of inflation, take out plated film after glass, be put into annealing furnace, 450 DEG C anneal 25 minutes take out.
2. a kind of ultraviolet 300nm as described in claim 1 is semi-transparent-and the preparation method of copper and indium doped transparent conductive film, feature Be, when resulting conductive film 300nm transmitance be greater than 50% when, then should extend plated film time.
3. a kind of ultraviolet 300nm as described in claim 1 is semi-transparent-preparation method of copper and indium doped transparent conductive film, feature Be, when resulting conductive film 300nm transmitance less than 50%, then should shorten plated film time or be appropriately extended annealing when Between.
4. a kind of ultraviolet 300nm is semi-transparent-copper and indium doped transparent conductive film, which is characterized in that by preparation side described in claim 1 Method preparation gained.
CN201810965660.1A 2018-08-23 2018-08-23 A kind of ultraviolet 300nm is semi-transparent-copper and indium doped transparent conductive film and preparation method thereof Pending CN108950482A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101841003A (en) * 2010-03-30 2010-09-22 鲁东大学 Double-layer structure deep-ultraviolet transparent conductive film and preparation method thereof
CN103993261A (en) * 2014-05-29 2014-08-20 江苏大学 Preparation method of transparent conductive thin film with grating structure
CN103993282A (en) * 2014-05-30 2014-08-20 天津大学 Double-layer transparent conducting thin film and preparation method thereof
JP2017137572A (en) * 2016-01-28 2017-08-10 三菱マテリアル株式会社 Laminate transparent conductive film, laminate wiring film, and production method of laminate wiring film
CN108220886A (en) * 2018-02-28 2018-06-29 张治国 A kind of preparation method of ITO texture transparent conductive film

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101841003A (en) * 2010-03-30 2010-09-22 鲁东大学 Double-layer structure deep-ultraviolet transparent conductive film and preparation method thereof
CN103993261A (en) * 2014-05-29 2014-08-20 江苏大学 Preparation method of transparent conductive thin film with grating structure
CN103993282A (en) * 2014-05-30 2014-08-20 天津大学 Double-layer transparent conducting thin film and preparation method thereof
JP2017137572A (en) * 2016-01-28 2017-08-10 三菱マテリアル株式会社 Laminate transparent conductive film, laminate wiring film, and production method of laminate wiring film
CN108220886A (en) * 2018-02-28 2018-06-29 张治国 A kind of preparation method of ITO texture transparent conductive film

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
张治国: "紫外波段高透过率铜铟掺杂SnO2薄膜的研究", 《物理学报》 *

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