CN105551579B - One kind can electrochromic multi-layer transparent electroconductive film and preparation method thereof - Google Patents
One kind can electrochromic multi-layer transparent electroconductive film and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to film and preparation method thereof, provide one kind can electrochromic multi-layer transparent electroconductive film and preparation method thereof, the multi-layer transparent electroconductive film includes the substrate set gradually from top to bottom, the first WO3Film layer, Ag conductive layer, W buffer layer and the 2nd WO3Film layer；Preparation method passes through reactive sputtering first and prepares the first WO on substrate3Film layer；Then respectively by d.c. sputtering and magnetron sputtering in the first WO3Thin-film surface prepares Ag conductive layer and W buffer layer；The 2nd WO is finally prepared in W film surface by reactive sputtering again3Film layer, the present invention is by optimization multi-layer transparent electroconductive film structure and preparation process, being prepared into using sputtering method can electrochromic multi-layer transparent electroconductive film, and the film has the high transmittance in visible-range, high conductivity, and have that transmission of visible light adjustable range is big, coloration efficiency is high, good cycling stability and advantages of environment protection.
Description
Technical field
The present invention relates to films and preparation method thereof more particularly to one kind can electrochromic Multilayer stack structure (stack
Structure) transparent conductive film and preparation method thereof.
Background technique
Transparent conductive film is that optical clear performance and electric conductivity are compounded in integrated photoelectric material, since it has
Excellent photoelectric characteristic becomes research hotspot in recent years and advanced subject, can be widely applied to solar battery, electroluminescent change
The fields such as color, LED, TFT, LCD and touch screen.Most common transparent conductive material is tin indium oxide (ITO), but due to indium
It the scarcity of metal and rapidly depletes, leads to the continuous soaring of cost, therefore be badly in need of finding the relatively inexpensive alternative materials of one kind.
Wherein dielectric-metal-medium (DMD) structure is because it is with excellent optics, electricity and architectural characteristic (such as close to metal material
High conductivity, it is seen that the high transmittance in optical range, relatively low thickness and high-flexibility), be considered as most potential
Electrically conducting transparent alternative materials.
WO3It is most common one kind dielectric thin-film material in DMD structure, is to find that earliest and most typical electrochromism is thin
Membrane material has many advantages, such as that fast response time and coloration efficiency are high, therefore WO3-Ag-WO3(WAW) structure can be used as electricity simultaneously
Off-color material and transparent conductive film are caused, so that the cost of electrochromic device be effectively reduced.The main side using vapor deposition at present
Method prepares WAW multi-layer film structure, but main problem be film and substrate binding force it is not strong, not can guarantee the durable of device
Property, and sputtering method can be effectively solved this problem because of its sedimentary energy with higher, it furthermore can using reactive sputtering
To use relatively inexpensive metal targets, thin film composition can also be controlled by adjusting sputtering technology.Sputtering method has
Fast filming, performance stablize, simple process and low cost, be suitble to large area production etc. advantages become WAW preparation grind
Study carefully hot spot.
But according to the working principle of DMD transparent conductive film, to obtain lower resistivity, it is desirable that dielectric layer have compared with
High surface work function, makes it match with metal conducting layer, forms anti-drag barrier, improves Carrier Injection Efficiency, finally reaches
To high carrier transport efficiency.WO3Work function with Ag is respectively 5.24eV and 4.4ev, can satisfy this requirement；However
Ag conductive layer is in reactive sputter-deposition WO3When, it is easy to be aoxidized to form Ag by energetic oxygen ionsxO, work function is about 5.47~
5.61eV forms surface potential barrier in interface, hinders Ag and WO3Between electron exchange, so that film be made to lose electric conductivity.Cause
And how to prepare WAW film using sputtering method becomes research emphasis of the invention.
Summary of the invention
It can electrochromic multi-layer transparent conductive thin the purpose of the present invention is to solve the shortcomings of the prior art providing one kind
Film and preparation method thereof realizes prepared by the sputtering method of WAW film by the structure optimization to WAW film.The skill that the present invention uses
Art scheme are as follows:
One kind can electrochromic multi-layer transparent electroconductive film, including substrate, the first WO set gradually from the bottom up3It is thin
Film layer, Ag conductive layer and the 2nd WO3Film layer, which is characterized in that the Ag conductive layer and the 2nd WO3W is additionally provided between film layer
Buffer layer.
Further, the first WO3Film layer, Ag conductive layer, W buffer layer and the 2nd WO3The thickness of film layer is respectively
45nm, 10~12nm, 2~3nm and 45nm.The substrate is standard electronic white glass.
Further, it is above-mentioned can electrochromic multi-layer transparent electroconductive film preparation method, comprising the following steps:
Step 1. prepares the first WO3Film layer: by vacuum chamber, being subsequently passed argon gas and adjust ar pressure, it
Radio-frequency power supply switch is opened afterwards, is passed through oxygen after target build-up of luminance, is adjusted argon gas and oxygen flow, fix vacuum room pressure,
It sets sputtering power and pre-sputter cleaning is carried out to W target, then go to substrate platen right above target, set sputtering time,
WO is deposited on substrate3Film；
Step 2. prepares Ag conductive layer: adjusting ar pressure, opens DC power supply switch later, adjust argon after target build-up of luminance
Throughput fixes vacuum room pressure, and setting sputtering power carries out pre-sputter cleaning to Ag target, then turns substrate platen
Right above to target, sputtering time is set, in the first WO3Ag film is deposited in film layer；
Step 3. prepares W buffer layer: adjusting ar pressure, opens radio-frequency power supply switch later, adjust argon after target build-up of luminance
Throughput fixes vacuum room pressure, and setting sputtering power carries out pre-sputter cleaning to W target, then turns substrate platen
Right above to target, sputtering time is set, deposits W film on Ag conductive layer；
Step 4. prepares the 2nd WO3Film layer: adjusting ar pressure, opens radio-frequency power supply later and switchs, after target build-up of luminance
It is passed through oxygen, argon gas and oxygen flow is adjusted, fixes vacuum room pressure, setting sputtering power carries out pre-sputtering to W target
Cleaning then goes to substrate platen right above target, sets sputtering time, deposits WO on W buffer layer3Film.
Further, in step 1, vacuumizing to vacuum chamber is carried out using mechanical pump and molecular pump, and vacuum chamber
Vacuum degree is evacuated to 2.0 × 10-4Pa~1.0 × 10-3Pa。
In step 1 and step 4, oxygen and argon flow are respectively 40sccm and 60sccm, rf sputtering power 200W,
Deposition rate is 2.5nm/min.
In step 2, argon flow 60sccm, sputtering power 10W, deposition rate 2Onm/min.
In step 3, argon flow 80sccm, sputtering power 200W, deposition rate l5nm/min.
The present invention provides substrate, the first WO3Film layer, Ag conductive layer, W buffer layer and the 2nd WO3The WO that film layer is constituted3-
Ag-W-WO3Stack architecture can electrochromic multi-layer transparent electroconductive film, and the work function of W is 4.55eV, very close Ag's
Work function, in Ag conductive layer and the 2nd WO3W metal buffer layer is inserted between film layer can be avoided the 2nd WO of sputtering preparation3Film
Destruction during layer to Ag metal conducting layer, while also can be used as work-function matching layer, promote electron-transport.
To sum up, the invention has the following advantages:
1) present invention can guarantee the high quality multi-layer thin for realizing substrate binding force height, even compact using magnetron sputtering technique
Film deposition；
2) present invention process and equipment are simple, easy, and using metal targets, low in cost, film growth rate is fast, are applicable in
In large-scale industrial production；
3) the multi-layer transparent electroconductive film electric conductivity prepared by the present invention is good, and light transmission adjustable range is big, coloring is imitated
Rate height, good cycling stability, in display device, dimming glass, the fields such as information storage have broad application prospects.
Detailed description of the invention
Fig. 1 be the present invention can electrochromic multi-layer transparent electroconductive film structural schematic diagram, wherein 1 be substrate, 2 be
First WO3Film layer, 3 be Ag conductive layer, 4 be W buffer layer, 5 be the 2nd WO3Film layer.
Fig. 2 is the transmission of the multi-layer transparent electroconductive film visible-range intrinsic color state that embodiment 1 is prepared into and bleaching state
Rate test curve figure.
Fig. 3 is the multi-layer transparent electroconductive film voltage and current loop test curve graph that embodiment 1 is prepared into.
Specific embodiment
Invention is further described in detail with attached drawing combined with specific embodiments below.
Embodiment 1
In the present embodiment provide can electrochromic multi-layer transparent electroconductive film, structure is as shown in Figure 1, include from lower past
On the substrate, the first WO that set gradually3Film layer, Ag conductive layer, W buffer layer and the 2nd WO3Film layer, the first WO3Film layer,
Ag conductive layer, W buffer layer and the 2nd WO3The thickness of film layer is respectively 45nm, 10~12nm, 2~3nm and 45nm, and substrate is adopted
With standard electronic white glass.
Preparation method includes the following steps:
1) the first WO is prepared3Film layer: by vacuum chamber (~5.0 × 10-4Pa), it is subsequently passed argon gas, adjusts argon
Gas air pressure (1.0Pa) opens radio-frequency power supply switch later, oxygen is passed through after target build-up of luminance, adjust argon gas and oxygen flow (40:
60sccm), vacuum room pressure is made to fix (4.0 × 10-1Pa), sputtering power (200W) is adjusted, W target is splashed in advance later
Cleaning (10 minutes) are penetrated, then go to substrate platen right above target, are adjusted sputtering time (18 minutes), on a glass substrate
Deposit WO3Film；
2) it prepares Ag conductive layer: adjusting argon flow (60sccm), vacuum room pressure is made to fix (3.4 × 10-1Pa), it
After open DC power supply switch, after target build-up of luminance, adjust sputtering power (10W), pre-sputter cleaning (5 carried out to Ag target later
Minute), then substrate platen is gone to right above target, is adjusted sputtering time (36 seconds), in the first WO3Ag is deposited in film layer
Film；
3) it prepares W buffer layer: adjusting ar pressure (1.0Pa), open radio-frequency power supply later and switch, after target build-up of luminance, adjust
It saves argon flow (80sccm), vacuum room pressure is made to fix (4.7 × 10-1Pa), sputtering power (200W) is adjusted, later to W
Target carries out pre-sputter cleaning (5 minutes), then goes to substrate platen right above target, adjusts sputtering time (8 seconds), in Ag
W film is deposited on conductive layer；
4) the 2nd WO is prepared3Film layer: being adjusted ar pressure (1.0Pa), opens radio-frequency power supply switch, target build-up of luminance later
After be passed through oxygen, adjust argon gas and oxygen flow (40:60sccm), vacuum room pressure made to fix (4.0 × 10-1Pa), adjust
Sputtering power (200W) then goes to substrate platen right above target, adjusts sputtering time (18 minutes), on W buffer layer
Deposit WO3Film.
To it is above-mentioned can electrochromic multi-layer transparent electroconductive film carry out emulation testing, result is as shown in Figure 2 and Figure 3, figure
2 transmission for the multi-layer transparent electroconductive film after visible-range intrinsic color state and bleaching state single and 2000 circulation conversions
Rate test curve comparison diagram.
Embodiment 2
Using following steps be prepared into the identical structure of embodiment 1 can electrochromic multi-layer transparent electroconductive film, specifically:
1) the first WO is prepared3Film layer: by vacuum chamber (~5.0 × 10-4Pa), it is subsequently passed argon gas, adjusts argon
Gas air pressure (1.0Pa) opens radio-frequency power supply switch later, oxygen is passed through after target build-up of luminance, adjust argon gas and oxygen flow (40:
60sccm), vacuum room pressure is made to fix (4.0 × 10-1Pa), sputtering power (200W) is adjusted, W target is splashed in advance later
Cleaning (10 minutes) are penetrated, then go to substrate platen right above target, are adjusted sputtering time (18 minutes), on a glass substrate
Deposit WO3Film；
2) it prepares Ag conductive layer: adjusting argon flow (60sccm), vacuum room pressure is made to fix (3.4 × 10-1Pa), it
After open DC power supply switch, after target build-up of luminance, adjust sputtering power (10W), pre-sputter cleaning (5 carried out to Ag target later
Minute), then substrate platen is gone to right above target, is adjusted sputtering time (30 seconds), in the first WO3Ag is deposited in film layer
Film；
3) it prepares W buffer layer: adjusting ar pressure (1.0Pa), open radio-frequency power supply later and switch, after target build-up of luminance, adjust
It saves argon flow (80sccm), vacuum room pressure is made to fix (4.7 × 10-1Pa), sputtering power (200W) is adjusted, later to W
Target carries out pre-sputter cleaning (5 minutes), then goes to substrate platen right above target, adjusts sputtering time (8 seconds), in Ag
W film is deposited on conductive layer；
4) the 2nd WO is prepared3Film layer: being adjusted ar pressure (1.0Pa), opens radio-frequency power supply switch, target build-up of luminance later
After be passed through oxygen, adjust argon gas and oxygen flow (40:60sccm), vacuum room pressure made to fix (4.0 × 10-1Pa), adjust
Sputtering power (200W) then goes to substrate platen right above target, adjusts sputtering time (18 minutes), on W buffer layer
Deposit WO3Film.
Embodiment 3
Using following steps be prepared into the identical structure of embodiment 1 can electrochromic multi-layer transparent electroconductive film, specifically:
1) the first WO is prepared3Film layer: by vacuum chamber (~5.0 × 10-4Pa), it is subsequently passed argon gas, adjusts argon
Gas air pressure (1.0Pa) opens radio-frequency power supply switch later, oxygen is passed through after target build-up of luminance, adjust argon gas and oxygen flow (40:
60sccm), vacuum room pressure is made to fix (4.0 × 10-1Pa), sputtering power (200W) is adjusted, W target is splashed in advance later
Cleaning (10 minutes) are penetrated, then go to substrate platen right above target, are adjusted sputtering time (18 minutes), on a glass substrate
Deposit WO3Film；
2) it prepares Ag conductive layer: adjusting argon flow (60sccm), vacuum room pressure is made to fix (3.4 × 10-1Pa), it
After open DC power supply switch, after target build-up of luminance, adjust sputtering power (10W), pre-sputter cleaning (5 carried out to Ag target later
Minute), then substrate platen is gone to right above target, is adjusted sputtering time (30 seconds), in the first WO3Ag is deposited in film layer
Film；
3) it prepares W buffer layer: adjusting ar pressure (1.0Pa), open radio-frequency power supply later and switch, after target build-up of luminance, adjust
It saves argon flow (80sccm), vacuum room pressure is made to fix (4.7 × 10-1Pa), sputtering power (200W) is adjusted, later to W
Target carries out pre-sputter cleaning (5 minutes), then goes to substrate platen right above target, adjusts sputtering time (9 seconds), in Ag
W film is deposited on conductive layer；
4) the 2nd WO is prepared3Film layer: being adjusted ar pressure (1.0Pa), opens radio-frequency power supply switch, target build-up of luminance later
After be passed through oxygen, adjust argon gas and oxygen flow (40:60sccm), vacuum room pressure made to fix (4.1 × 10-1Pa), adjust
Sputtering power (200W) then goes to substrate platen right above target, adjusts sputtering time (18 minutes), on W buffer layer
Deposit WO3Film.
The above description is merely a specific embodiment, any feature disclosed in this specification, except non-specifically
Narration, can be replaced by other alternative features that are equivalent or have similar purpose；Disclosed all features or all sides
Method or in the process the step of, other than mutually exclusive feature and/or step, can be combined in any way.
Claims (1)
1. one kind can electrochromic multi-layer transparent electroconductive film, including substrate, the first WO set gradually from the bottom up3Film
Layer, Ag conductive layer, W buffer layer and the 2nd WO3Film layer, the first WO3Film layer, Ag conductive layer, W buffer layer and the 2nd WO3Film
The thickness of layer is respectively 45nm, 10~12nm, 2~3nm and 45nm, and substrate uses standard electronic white glass；
It is described can electrochromic multi-layer transparent electroconductive film preparation method the following steps are included:
1) the first WO is prepared3Film layer: by vacuum chamber to 5.0 × 10-4Pa is subsequently passed argon gas, adjusts ar pressure
For 1.0Pa, radio-frequency power supply switch is opened later, is passed through oxygen after target build-up of luminance, adjusting argon gas and oxygen flow is 40:
60sccm makes vacuum room pressure be fixed as 4.0 × 10-1Pa, adjusting sputtering power are 200W, are splashed in advance to W target later
Cleaning 10 minutes is penetrated, then goes to substrate platen right above target, adjusting sputtering time is 18 minutes, is sunk on a glass substrate
Product WO3Film；
2) prepare Ag conductive layer: adjusting argon flow is 60sccm, and vacuum room pressure is made to be fixed as 3.4 × 10-1Pa is beaten later
Open DC power supply switch, after target build-up of luminance, adjusting sputtering power is 10W, Ag target is carried out pre-sputter cleaning 5 minutes later,
Then substrate platen is gone to right above target, adjusting sputtering time is 36 seconds, in the first WO3Ag film is deposited in film layer；
3) prepare W buffer layer: adjusting ar pressure is 1.0Pa, opens radio-frequency power supply later and switchs, and after target build-up of luminance, adjusts argon
Throughput is 80sccm, and vacuum room pressure is made to be fixed as 4.7 × 10-1Pa, adjusting sputtering power is 200W, later to W target
It carries out pre-sputter cleaning 5 minutes, then goes to substrate platen right above target, adjust sputtering time 8 seconds, on Ag conductive layer
Deposit W film；
4) the 2nd WO is prepared3Film layer: adjusting ar pressure is 1.0Pa, opens radio-frequency power supply switch later, leads to after target build-up of luminance
Enter oxygen, adjusts argon gas and oxygen flow 40:60sccm, vacuum room pressure is made to be fixed as 4.0 × 10-1Pa adjusts sputtering function
Rate is 200W, then goes to substrate platen right above target, and adjusting sputtering time is 18 minutes, deposits WO on W buffer layer3
Film.
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| CN106848104B (en) * | 2017-04-14 | 2019-07-26 | 京东方科技集团股份有限公司 | Top emission type luminescent device |
| CN107604334A (en) * | 2017-09-21 | 2018-01-19 | 中国建筑材料科学研究总院 | Nickel-tungsten oxide film and preparation method thereof |
| US10187107B1 (en) * | 2018-04-23 | 2019-01-22 | Nokia Solutions And Networks Oy | Electrochromic switch |
| US10446746B1 (en) | 2018-05-01 | 2019-10-15 | International Business Machines Corporation | ReRAM structure formed by a single process |
| CN108786807A (en) * | 2018-06-19 | 2018-11-13 | 陕西科技大学 | A kind of graphene/WO3The preparation of/Ag composite photocatalysis films |
| CN112210754B (en) * | 2020-08-31 | 2022-12-06 | 基迈克材料科技（苏州）有限公司 | Preparation method of electrochromic film system and preparation method of electrochromic device |
| CN113549882B (en) * | 2021-06-03 | 2022-06-14 | 电子科技大学 | Preparation method of tungsten trioxide nanowire electrochromic film |
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| CN1363530A (en) * | 2001-01-09 | 2002-08-14 | 上海耀华皮尔金顿玻璃股份有限公司 | Absorption-type low-radiation film coated glass |
| CN101509126A (en) * | 2009-03-18 | 2009-08-19 | 王凯 | Apparatus and method for producing transparent conductive oxide film |
| CN102013294A (en) * | 2010-09-10 | 2011-04-13 | 东莞市福德电子有限公司 | High-resistance value metal oxide film resistor and manufacture method thereof |
| CN104766894A (en) * | 2015-04-08 | 2015-07-08 | 合肥工业大学 | Method for improving photoelectric property of dielectric/metal/dielectric electrodes |
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