CN106637078A - Film manufacturing method - Google Patents
Film manufacturing method Download PDFInfo
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- CN106637078A CN106637078A CN201611076621.3A CN201611076621A CN106637078A CN 106637078 A CN106637078 A CN 106637078A CN 201611076621 A CN201611076621 A CN 201611076621A CN 106637078 A CN106637078 A CN 106637078A
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- Prior art keywords
- substrate
- flow
- film
- ito
- substep
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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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
-
- 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
Abstract
The invention discloses a film manufacturing method. The film manufacturing method includes the following steps that a substrate is provided and heated, the substrate is maintained to be at 230 DEG C to 300 DEG C, and an ITO film is manufactured on the substrate in the atmosphere of reduction gas; before the ITO film deposition step is executed, only Ar gas is led in, and the flow is 0; and in the first stage of ITO film deposition, the flow is increased step by step and is increased to the maximum degree from 0. According to the film manufacturing method, the ITO film is manufactured in the atmosphere of reduction gas, In and Sn oxide saturation state and non-saturation state coexisting solid solution multicrystal film is generated, the ITO film is controlled to grow in the direction facilitating surface roughness improving, and the aim of improving the surface roughness of the ITO film is achieved.
Description
Technical field
The present invention relates to a kind of film, specifically a kind of preparation method of film.
Background technology
For resistive touch screen, no matter using G+G (Glass+Glass) structures or using F+G (Film+
Glass) structure, the resistance on touch-screen ITO Film and ito glass is all very high, and ito thin film is very thin, and its surface roughness compares
It is low, it is required for a small amount of temporal separation, i.e. touch-control to there is certain holdup time after touch-control terminates, affect touch-control response speed.
Meanwhile, G+G structural formulas touch-screen can send in fluctuating plate glass contact moment " " sound, some producers of this sound are referred to as different
Sound, seems especially prominent where night or peace and quiet.So touch-screen producer is it is generally desirable to the ITO of touch screens ito glass
The surface roughness of film is the bigger the better, particularly the resistive touch screen of G+G structures, the table of the ito thin film of upper and lower sheet glass
Surface roughness is higher, and touch-control is more beneficial to the separation between surface conductive glass and bottom electro-conductive glass after terminating, improve touch-screen
Response speed.Meanwhile, when the roughness ratio of two sheet glass is larger, presses watch crystal and there is no abnormal sound in glass contact
Sound, feels more preferably so as to experience.At present, in order to improve surface roughness, employ glass is polished, chemical method corrosion glass
Glass surface or the method for sandblasting, it is tactile so as to be lifted by the response speed for lifting the roughness of glass substrate to lift touch-screen
Control experience.However, although the mode of existing polishing, chemical attack or sandblasting can improve the surface roughness of glass surface,
The surface roughness of ito thin film cannot be improved.Meanwhile, increase above procedure and all will further improve production cost, crush spread
Space, is unfavorable for scheduling of production, cost efficiency, is also unfavorable for the operating profit of lifting company.
The content of the invention
It is an object of the invention to provide a kind of preparation method of film, to solve above-mentioned background technology in propose ask
Topic.
For achieving the above object, the present invention provides following technical scheme：
A kind of preparation method of film, comprises the steps：Substrate is provided, the substrate is heated, and by the substrate
Maintain 230～300 DEG C, in reducibility gas atmosphere, prepare ito thin film over the substrate, ito thin film deposition step it
Before, only leading to Ar gas, flow is 0, the first stage of ito thin film deposition, O2Flow substep increases, and from 0 maximum is increased to always.
As further scheme of the invention：Described the step of prepare ito thin film is over the substrate splashed using magnetic control
Penetrate and prepare over the substrate ito thin film.
As further scheme of the invention：The offer substrate, heats to the substrate, and the substrate is tieed up
Hold the step of 230～300 DEG C is that the substrate is maintained into 260～270 DEG C.
As further scheme of the invention：The second stage of the ito thin film deposition, O2Flow substep reduces, by most
Big value is gradually decreased to 0.
As further scheme of the invention：In O2During flow substep increases or substep reduces, the substep time is
3s～8s；Substep O2Flow is 0.05～0.2sccm.
As further scheme of the invention：O2Flow increases in arithmetic progression substep or substep reduces.
As further scheme of the invention：The second stage of the ito thin film deposition, in O2Flow substep reduces it
Before, also including transition step, O in the transition step2Flow keeps maximum constant.
As further scheme of the invention：It is 10s that the flow is kept for the maximum constant time.
Compared with prior art, beneficial effects of the present invention O2It is：It is thin that the present invention prepares ITO in reducibility gas atmosphere
Film, generates the polycrystal membrane of the solid solution that In, Sn oxide saturated mode and unsaturated state coexist, and control ito thin film is to favourable
In the direction growth for improving surface roughness, the purpose of the surface roughness of raising ito thin film is realized.
Specific embodiment
The technical scheme in the embodiment of the present invention is clearly and completely described below.
In the embodiment of the present invention, a kind of preparation method of film comprises the steps：Substrate is provided, the substrate is entered
Row heating, and the substrate is maintained into 230～300 DEG C, in reducibility gas atmosphere, ITO is prepared over the substrate thin
Film, before ito thin film deposition step, only leads to Ar gas, O2Flow is 0, the first stage of ito thin film deposition, O2Flow substep increases
Plus, increase to maximum always from 0.Described is described the step of prepare ito thin film over the substrate using magnetron sputtering
Ito thin film is prepared on substrate.The offer substrate, heats to the substrate, and the substrate is maintained into 230～300
DEG C the step of be that the substrate is maintained into 260～270 DEG C.The second stage of the ito thin film deposition, O2Flow substep subtracts
It is little, it is gradually decreased to 0 by maximum.In O2During flow substep increases or substep reduces, the substep time is 3s～8s；Point
Step O2Flow is 0.05～0.2sccm.O2Flow increases in arithmetic progression substep or substep reduces.The of ito thin film deposition
Two-stage, in O2Before flow substep reduces, also including transition step, O in the transition step2Flow keeps maximum constant.
The O2It is 10s that flow is kept for the maximum constant time.
Substrate is selected as needed.When needing for ito thin film to be applied to LCD, resistive touch screen or capacitive touch screen
When, substrate is generally glass substrate.Substrate is cleaned first, and substrate is heated after being dried, and substrate is maintained
To 230～300 DEG C.In reducibility gas atmosphere, ito thin film is prepared on substrate, wherein, reducibility gas selected from hydrogen,
One kind in vapor and carbon monoxide, or the gas mixture of the mixed gas selected from argon gas and hydrogen, argon gas and vapor
And the one kind in the gas mixture of argon gas and carbon monoxide.Ito thin film can be prepared on substrate using magnetron sputtering.Also
In originality atmosphere prepare ITO films, using reducibility gas adjust ito thin film in In, Sn degree of oxidation and generate not
Isomorphous region feature peak, realizes the purpose of the surface roughness of raising ito thin film.
The flow of reducibility gas is too low, then be difficult to reach the effect of the roughness for improving ito thin film；And reducibility gas
Flow it is too high, then In, Sn metal aggregation phenomenon in ito thin film can be made excessively obvious, so as to the transmitance of product is too low and difficult
To meet transmitance needs, and reproducibility gas content is too high In and Sn metal whiskers also easily occurs, sees under special light
Examining can find blue mist phenomenon, and ito film layer resistance is affected Jing after wiping, and affect using effect.
Embodiment 1
0.7mm glass substrates are provided, and glass substrate is cleaned, then glass is loaded into coating wire, using coating wire
Heater is gradually heated to 270 DEG C in glass traveling process to glass substrate, and maintains 270 DEG C.2nd, ITO films are prepared
When be passed through NO2 as oxidizing gas, in oxidizing gas atmosphere, adopt magnetic control splash prepare on a glass substrate transmitance for
93%th, resistance range is 400～600 ohm of the high TP-400 ohm ito glasses thoroughly of resistive touch screen.Wherein, the stream of NO2
Measure as 0.6sccm, using Ar as process gas, the flow of Ar is 120sccm, and the voltage of magnetron sputtering is 312V, and power is
1.85kw, plated film beat is 150s.Adopt Shimadzu production UV2450 spectrophotometric determination ito thin films light transmittance for >=
93%.Adopt Guangzhou semiconductor to produce the probe machine of SDY-5 types four and determine the surface resistance of prepared ito thin film for 478～505
Ohm, the product for preparing normally is packed, and is positioned over normal humiture (temperature≤25 DEG C, the storehouse of the control of humidity≤60%)
Place in storehouse, and deposit 2 days, 7 days, 15 days in warehouse, then the surface resistance that identical method determines ito thin film is respectively adopted, knot
Fruit is 475～513 ohm.The product is cleaned, it is harsh and fit into after TP finished products with ITO Film, then tear ITO
Film, tests ito glass surface resistance, is as a result 468～523 ohm.It can be seen that, the resistance of the ito thin film prepared using the method
It is very stable, it is to avoid by traditional method provide that resistance value makes resistance value subsequently reduce naturally and bring when preparing it is equal
The problem of even property difference.
Embodiment 2
0.55mm glass substrates are provided, and glass substrate are cleaned and is dried, then glass substrate is carried out to be heated to 250
DEG C, and maintain 250 DEG C.2nd, vapor is passed through as reducibility gas, in reducibility gas atmosphere, existed using magnetron sputtering
Transmitance more than 90%, the general T P ito glass of 400～600 ohm of resistance are prepared in glass substrate.Wherein, vapor
Flow is 6sccm, and using Ar as process gas, the flow of Ar is 120sccm, and the voltage of magnetron sputtering is 327V, and power is
3.15kw, plated film beat is 56s.The light transmittance of Shimadzu production UV2450 spectrophotometric determination ito thin films is adopted for >=90%.
The XE-100 AFMs manufactured using PSIA companies test the surface roughness Ra >=0.8nm of ito thin film.Except not existing
Carry out in reducibility gas atmosphere beyond plated film, ito thin film is prepared by above-mentioned identical gas technology, using identical measure side
Method determines the surface roughness Ra≤0.4nm of ito thin film.It can be seen that, the ito thin film prepared in reducing atmosphere, it is possible to increase
The surface roughness of ito thin film.
Embodiment 3
0.5mm glass substrates are provided, and glass substrate is cleaned, then glass is loaded into coating wire, using coating wire
Heater is gradually heated to 250 DEG C in glass traveling process to glass substrate, and maintains 250 DEG C.2nd, ITO films are prepared
When be passed through NO2 as oxidizing gas, in oxidizing gas atmosphere, adopt magnetic control splash prepare on a glass substrate transmitance for
93%th, resistance is 500 ohm of the high TP-400 ohm ito glasses thoroughly of resistive touch screen.Wherein, the flow of NO2 is
0.6sccm, using Ar as process gas, the flow of Ar is 120sccm, and the voltage of magnetron sputtering is 312V, and power is
1.85kw, plated film beat is 150s.Adopt Shimadzu production UV2450 spectrophotometric determination ito thin films light transmittance for >=
93%.Adopt Guangzhou semiconductor to produce the probe machine of SDY-5 types four and determine the surface resistance of prepared ito thin film for 478～505
Ohm, the product for preparing normally is packed, and is positioned over normal humiture (temperature≤25 DEG C, the storehouse of the control of humidity≤60%)
Place in storehouse, and deposit 2 days, 7 days, 15 days in warehouse, then the surface resistance that identical method determines ito thin film is respectively adopted, knot
Fruit is 500 ohm.The product is cleaned, it is harsh and fit into after TP finished products with ITO Film, then tear ITO Film, survey
Examination ito glass surface resistance, is as a result 480 ohm.It can be seen that, the resistance of the ito thin film prepared using the method is very stable, it is to avoid
The problem of the lack of homogeneity that resistance value makes resistance value subsequently reduce naturally and brings is provided by traditional method when preparing.
Embodiment 4
0.68mm glass substrates are provided, and glass substrate are cleaned and is dried, then glass substrate is carried out to be heated to 280
DEG C, and maintain 280 DEG C.2nd, vapor is passed through as reducibility gas, in reducibility gas atmosphere, existed using magnetron sputtering
Transmitance more than 90%, the general T P ito glass of 480 ohm of resistance are prepared in glass substrate.Wherein, the flow of vapor is
6sccm, using Ar as process gas, the flow of Ar is 120sccm, and the voltage of magnetron sputtering is 327V, and power is 3.15kw,
Plated film beat is 56s.The light transmittance of Shimadzu production UV2450 spectrophotometric determination ito thin films is adopted for >=90%.Using
The XE-100 AFMs of PSIA companies manufacture test the surface roughness Ra >=0.8nm of ito thin film.Except not in reduction
Property atmosphere in carry out beyond plated film, prepare ito thin film by above-mentioned identical gas technology, using identical assay method survey
Determine the surface roughness Ra≤0.4nm of ito thin film.It can be seen that, the ito thin film prepared in reducing atmosphere, it is possible to increase ITO is thin
The surface roughness of film.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of spirit or essential attributes without departing substantially from the present invention, the present invention can be in other specific forms realized.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit is required rather than described above is limited, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.Moreover, it will be appreciated that although this specification is been described by according to embodiment, not each
Embodiment only includes an independent technical scheme, and this narrating mode of specification is only this area for clarity
Technical staff should using specification as an entirety, the technical scheme in each embodiment can also Jing it is appropriately combined, form this
Art personnel may be appreciated other embodiment.
Claims (8)
1. a kind of preparation method of film, it is characterised in that comprise the steps：Substrate is provided, the substrate is heated,
And the substrate is maintained into 230～300 DEG C, and in reducibility gas atmosphere, ito thin film is prepared over the substrate, ITO is thin
Before film deposition step, only lead to Ar gas, flow is 0, the first stage of ito thin film deposition, flow substep increases, and increases always from 0
It is added to maximum.
2. the preparation method of film according to claim 1, it is characterised in that described to prepare ITO over the substrate thin
The step of film is to prepare ito thin film over the substrate using magnetron sputtering.
3. the preparation method of film according to claim 1, it is characterised in that the offer substrate, enters to the substrate
The step of going and heat, and the substrate is maintained into 230～300 DEG C is that the substrate is maintained into 260～270 DEG C.
4. the preparation method of film according to claim 1, it is characterised in that the second stage of the ito thin film deposition,
Flow substep reduces, and by maximum 0 is gradually decreased to.
5. the preparation method of film according to claim 1, it is characterised in that increase in flow substep or substep reduces
During, the substep time is 3s～8s；Substep O2Flow is 0.05～0.2sccm.
6. the preparation method of film according to claim 1, it is characterised in that O2Flow in arithmetic progression substep increase or
Substep reduces.
7. the preparation method of film according to claim 1, it is characterised in that the second stage of the ito thin film deposition,
In O2Before flow substep reduces, also including transition step, O in the transition step2Flow keeps maximum constant.
8. the preparation method of film according to claim 7, it is characterised in that the O2Flow keeps maximum constant
Time is 10s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611076621.3A CN106637078A (en) | 2016-11-30 | 2016-11-30 | Film manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611076621.3A CN106637078A (en) | 2016-11-30 | 2016-11-30 | Film manufacturing method |
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|---|---|
| CN106637078A true CN106637078A (en) | 2017-05-10 |
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ID=58813194
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611076621.3A Pending CN106637078A (en) | 2016-11-30 | 2016-11-30 | Film manufacturing method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108183137A (en) * | 2017-12-28 | 2018-06-19 | 中国科学院电工研究所 | Composite conducting antireflective film for silicon/crystalline silicon heterojunction solar cell and preparation method thereof |
| CN110453175A (en) * | 2019-08-22 | 2019-11-15 | 中国科学院微电子研究所 | A kind of preparation method of vanadium oxide film |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020034836A1 (en) * | 2000-07-25 | 2002-03-21 | Nippon Sheet Glass Co., Ltd. | Method of manufacturing substrate having transparent conductive film, substrate having transparent conductive film manufactured using the method, and touch panel using the substrate |
| CN104109838A (en) * | 2014-07-04 | 2014-10-22 | 宜昌南玻显示器件有限公司 | ITO film and preparation method thereof |
| CN104109839A (en) * | 2014-07-04 | 2014-10-22 | 宜昌南玻显示器件有限公司 | ITO film and preparation method thereof |
| CN104164654A (en) * | 2014-07-23 | 2014-11-26 | 华灿光电股份有限公司 | Method for preparing transparent conductive film |
| CN104651785A (en) * | 2013-11-18 | 2015-05-27 | 北京北方微电子基地设备工艺研究中心有限责任公司 | A preparing method of an ITO film |
-
2016
- 2016-11-30 CN CN201611076621.3A patent/CN106637078A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020034836A1 (en) * | 2000-07-25 | 2002-03-21 | Nippon Sheet Glass Co., Ltd. | Method of manufacturing substrate having transparent conductive film, substrate having transparent conductive film manufactured using the method, and touch panel using the substrate |
| CN104651785A (en) * | 2013-11-18 | 2015-05-27 | 北京北方微电子基地设备工艺研究中心有限责任公司 | A preparing method of an ITO film |
| CN104109838A (en) * | 2014-07-04 | 2014-10-22 | 宜昌南玻显示器件有限公司 | ITO film and preparation method thereof |
| CN104109839A (en) * | 2014-07-04 | 2014-10-22 | 宜昌南玻显示器件有限公司 | ITO film and preparation method thereof |
| CN104164654A (en) * | 2014-07-23 | 2014-11-26 | 华灿光电股份有限公司 | Method for preparing transparent conductive film |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108183137A (en) * | 2017-12-28 | 2018-06-19 | 中国科学院电工研究所 | Composite conducting antireflective film for silicon/crystalline silicon heterojunction solar cell and preparation method thereof |
| CN108183137B (en) * | 2017-12-28 | 2019-10-15 | 中国科学院电工研究所 | Composite conducting antireflective film and preparation method thereof for silicon/crystalline silicon heterojunction solar cell |
| CN110453175A (en) * | 2019-08-22 | 2019-11-15 | 中国科学院微电子研究所 | A kind of preparation method of vanadium oxide film |
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