CN109872834A - A kind of electrically conducting transparent silver grid film and preparation method thereof - Google Patents
A kind of electrically conducting transparent silver grid film and preparation method thereof Download PDFInfo
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- CN109872834A CN109872834A CN201910315144.9A CN201910315144A CN109872834A CN 109872834 A CN109872834 A CN 109872834A CN 201910315144 A CN201910315144 A CN 201910315144A CN 109872834 A CN109872834 A CN 109872834A
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Abstract
The present invention relates to thin-film material technical fields more particularly to a kind of electrically conducting transparent silver grid film and preparation method thereof.The electrically conducting transparent grid film is prepared by no particle silver ink water, including the irregular grid to extend in in-plane being made by silver-colored grid lines, including conduction region and insulation layer, conduction region is the grid frame in irregular shape that silver-colored grid lines is made into, insulation layer is the white space that silver-colored grid lines impales, electrically conducting transparent silver grid film film thickness is 2-20 μm, transmitance is 60~92%, square resistance is 1-50 Ω/sq, no particle silver ink water is coated on the cracked plate by the production of acrylic resin CA-600 lotion by the present invention, the electrically conducting transparent silver grid film is obtained after drying process and cleaning.Network has preferable flexibility and electric conductivity in the present invention, is amenable to repeatedly bend and bend, and can get different grid patterns by setting spin coating proceeding parameter, and then obtain the conductive film with different transmitances and different square resistances.
Description
Technical field
The present invention relates to thin-film material technical field more particularly to a kind of electrically conducting transparent silver grid film and its preparation sides
Method.
Background technique
Transparent conductive film is that optical transparence and electric conductivity are compounded in integrated photoelectric material, has high light transmittance
Rate and high conductivity are widely used in such as OLED, flat-panel monitor, touch screen, transparent conductive electrode (TCE), transparent electromagnetic wave
It is cured with the biology such as such as skin prosthese sensor, intelligent invisible glasses in the electronics and information industries such as shielding material, transparent heater field
Field, wherein the very important application of transparent conductive film first is that transparent conductive electrode (TCE), tin indium oxide (ITO) are
The most mature material of TCE is made, has excellent electrical and optical performance, but the finiteness of indium metal, scarcity lead to ITO
The production cost increases for coated substrate, and it is right that the requirement for ITO electric conductivity and brittle heat treatment needed for obtaining limits its
The applicability of temperature sensitive flexible base board.In addition, development in science and technology and continuous improvement of people's living standards with rapid changepl. never-ending changes and improvements promotees
Make the fast development of intelligent movable equipment, transparent conductive film market it is swift and violent increase but also following electronic equipment towards
The directions such as more intelligent, wearable, more frivolous are developed, and the device that traditional ito thin film has been unable to satisfy present wearableization is wanted
It asks, it is also imperative to the research of the next-generation transparent material of substitution ITO.
The free electron with high concentration makes metal-base film material have high electrical conductivity, metal inside metal material
The metal material used in base transparent conducting film material includes metal nanowire thin-films and metal grill film.Nano wire is transparent
The numerous characteristics for the nanowire structure that conductive film is constituted such as length, diameter, size, dispersibility and universe network form are all
It will affect performance, wherein the length and diameter of line is that nano wire transparent conductive film realizes the low haze, high grade of transparency, highly conductive
The key of property and excellent mechanical flexibility and intensity, but this is generally difficult to realize simultaneously and nano wire cannot be steady on base material
Fixed to exist, the network structure roughness of formation is big, and nano wire is very easy to gather into bundles, and dispersibility is low.
Summary of the invention
(1) technical problems to be solved
Big in order to solve nano wire transparent conductive film network roughness in the prior art, nano wire is very easy to poly-
Collect bunchy, the problems such as dispersibility is low, the present invention provides a kind of electrically conducting transparent silver grid with high light transmittance and high conductivity
Film and the preparation method that can be control effectively to the line width mesh of metallic silver network in the film.
(2) technical solution
In order to achieve the above object, the main technical schemes that the present invention uses include:
The present invention provides a kind of electrically conducting transparent silver grid films, and the electrically conducting transparent grid film is by no particle silver ink water system
Standby to form, including the irregular grid to extend in in-plane being made by silver-colored grid lines, these grids constitute conduction region and absolutely
Edge area, the conduction region are the grid frame in irregular shape that silver-colored grid lines is made into, and the insulation layer is that silver-colored grid lines impales
White space.
According to the present invention, which is 2-20 μm, and transmitance is 60~92%, square resistance
For 1-50 Ω/sq.
The present invention also provides a kind of electrically conducting transparent silver grid method for manufacturing thin film, the preparation method the following steps are included:
S1: it coats in crackle plate surface without particle silver ink water, is dried, obtains silver-colored grid film；
S2: the silver-colored grid film that step S1 is obtained is cleaned by ultrasonic, and finally obtains electrically conducting transparent silver grid film.
According to the present invention, the cracked plate is coated in substrate surface by crackle liquid, is made after being dried；
The crackle liquid is selected from water soluble acrylic resin CA-600 lotion, TiO2Colloidal sol, SiO2Colloidal sol, crackle nail polish,
Any one of egg white and ice template.
According to the present invention, TiO2Sol preparation step is as follows:
S11, by diethanol amine (DEA) and dehydrated alcohol (C2H5OH it) mixes, by butyl titanate (Ti after mixing
(OC4H9)4) be slowly dropped into form solution A；
S12, deionized water and dehydrated alcohol are mixed to form B solution；
S13, respectively by A, B solution utilize magnetic stirrer 1-3h；
S14, B solution is slowly added to be stirred for 1-3h in A, ultimately forms colloidal sol；
Ti(OC4H9)4With H2The molar ratio of O is 0.25-4；
C2H5The molar ratio of OH and DEA is 6.6-60.
According to the present invention, SiO also can be selected in the crackle liquid2Any in colloidal sol, crackle nail polish, egg white and ice template
Kind；
Described matrix is selected from glass, polyethylene terephthalate (PET), polyimides (PI), poly dimethyl silicon
Any one of oxygen alkane (PDMS) and phase paper base plate.
According to the present invention, the crackle liquid is in the coating method of substrate surface, the no particle silver ink water in the crackle
The coating method of plate surface is spin coating, in the spin coating process spin coating parameters be even painting revolving speed 500rpm, even painting time 15s,
Spin coating revolving speed is 1000-5000rpm, spin-coating time 20s.
According to the present invention, the crackle liquid is in the coating method of substrate surface, the no particle silver ink water in the crackle
The coating method of plate surface is drop coating, spraying, blade coating or magnetron sputtering.
According to the present invention, the drying process of the crackle liquid and the no particle silver ink water is dry using heating plate or vacuum
Dry case, heating rate are set as 40-200 DEG C/h, and drying temperature is set as 100-250 DEG C, soaking time 0.5-2h, after be down to furnace
Room temperature.
According to the present invention, in step s 2, the ultrasonic cleaning agent is that dehydrated alcohol or dehydrated alcohol and deionized water are mixed
Solution is closed, the ultrasonic cleaning time is set as 3-10min.
(3) beneficial effect
The beneficial effects of the present invention are:
Grid interconnected in the present invention in substrate will not mutually " bridging ", and regular metal grill can be ideally
The dense distribution of seepage flow, the contact resistance at grid knot and conducting wire between elimination conducting wire, network have lesser curvature
Radius meets the requirement of flexibility, has preferable flexibility as the flexible transparent conductive film of representative using metal grill and leads
Electrically, it is amenable to repeatedly bend and bend, can form a film at room temperature.The preparation side of electrically conducting transparent silver grid film in the present invention
Method is at low cost and does not need precision instrument, and raw material can be directly commercially available, and method is simple and environmentally-friendly.
Detailed description of the invention
Fig. 1 is the conduction region and insulation layer structural schematic diagram of electrically conducting transparent silver grid film of the present invention；
Fig. 2 is the different line widths of the embodiment of the present invention 1 and the crackle template shape appearance figure of mesh quantity；
Fig. 3 is electrically conducting transparent silver grid membrane structure schematic diagram made from the embodiment of the present invention 1；
Fig. 4 is the transmittance curve comparison diagram of electrically conducting transparent silver grid film under 1 different rotating speeds of the embodiment of the present invention；
Fig. 5 is the crackle template sectional view of different-thickness made from the embodiment of the present invention 2；
Fig. 6 is TiO in the embodiment of the present invention 32The crack morphology figure of colloidal sol cracked plate；
Fig. 7 is 3 difference TiO of the embodiment of the present invention2The transmitance of electrically conducting transparent silver grid film made from colloidal sol density is bent
Line comparison diagram.
Specific embodiment
In order to preferably explain the present invention, in order to understand, with reference to the accompanying drawing, by specific embodiment, to this hair
It is bright to be described in detail.
The present invention provides a kind of electrically conducting transparent silver grid film with high light transmittance and high conductivity and its preparation sides
Method.
The electrically conducting transparent silver grid film includes the irregular grid to extend in in-plane being made by silver-colored grid lines, institute
Stating grid composition has conduction region and insulation layer, and wherein conduction region is the grid frame being made by silver-colored grid lines in irregular shape,
Insulation layer is the white space that silver-colored grid lines impales, and specific structure is as shown in Figure 1.
Conductive metal silver in the silver-colored grid lines of conduction region is prepared using the sintering of no particle conductive silver ink, the nothing
Grain conductive silver ink preparation method is simple and environmentally-friendly, low in cost, wherein be a kind of colorless and transparent stablizing solution without particle silver ink water,
The solution is made of silver-colored precursor compound, complex compound, solvent, surfactant and other auxiliary agents and filters and obtain through filter paper
It arrives, the silver-colored precursor compound is the mixing of one or more of silver citrate, silver acetate, silver tartrate, silver carbonate；
The complex compound is can to can be ethylenediamine, propane diamine, fourth two with the aminated compounds of the raw complex reaction ligand of silver hair
The mixing of one or more of amine, isopropylamine；The solvent is liquid alcohol compound, can be ethyl alcohol, methanol, isopropanol
One or more of mixing；The surfactant can be polyethylene Topiramate Los oxazolidinone, one in dodecyl sodium sulfate
Kind；The auxiliary agent can be one of polyethylene glycol, ethyl cellulose；The filtering, which refers to, passes through reaction solution
0.22~0.45 μm of membrane filtration purifying；Stablizing without particle silver inks water chemistry property for preparation, is easy storage, is unlikely to deteriorate,
Low-temperature sintering temperature is at 90~200 DEG C；The coating method has drop coating, spin coating, stick painting, spraying, blade coating, inkjet printing, silk
Wire mark brush and magnetron sputtering etc..
The present invention also provides a kind of preparation method for preparing electrically conducting transparent silver grid film without particle silver ink water with this,
The method for manufacturing thin film specifically includes the following steps:
S1: choosing crackle liquid, and take and be coated on matrix in right amount, obtains cracked plate after controlling temperature condition.
Selected crackle liquid needs to have the characteristic for being easy cracking by certain processing, such as acrylic resin CA-600
Lotion, TiO 2 sol, silicon dioxide gel, crackle nail polish, egg white and ice template etc..
Glass, polyethylene terephthalate (PET), polyimides (PI), poly dimethyl silicon can be used in described matrix
Oxygen alkane (PDMS), phase paper base plate etc..
In step sl, the appropriate crackle liquid is 20-100 μ L.
In step sl, the crackle liquid substrate surface coating processing can be selected drop coating, spin coating, spraying, blade coating or
Person's magnetron sputtering.
In step sl, the control temperature condition is to be dried using heating plate or vacuum oven, is heated up
Rate is set as 60-200 DEG C/h, and final cracked plate drying temperature is set as 100-250 DEG C, soaking time 0.5-2h, after make
It is down to room temperature with furnace.
S2: no particle silver ink water is coated in the crackle plate surface that step S1 is obtained, the two, which combines, makes no particle silver ink water
It penetrates into crackle, silver-colored grid film is obtained after drying process.
In step s 2, it is described be dried use heating plate or vacuum oven, heating rate be set as 40-200 DEG C/
H, final template drying temperature are set as 100-250 DEG C, soaking time 0.5-2h, after so that it is down to room temperature with furnace.
In step s 2, drop coating, spin coating, spray also can be used in the coating processing of crackle plate surface in the no particle silver ink water
Painting, blade coating or magnetron sputtering.
S3: the silver metal film that step S2 is obtained being put into supersonic cleaning machine and is cleaned, and is cleared up after removing cracked plate
Surface obtains electrically conducting transparent silver grid film.
In step s3, the ultrasonic cleaning agent in the supersonic cleaning machine is dehydrated alcohol or a certain proportion of anhydrous second
Pure and mild deionized water mixed solution, ultrasonic cleaning time are set as 2-10min, obtain the silver-colored grid film only deposited in substrate.
The electrically conducting transparent silver grid film film thickness be 2-20 μm, transmitance be 60~92%, square resistance be 1-50 Ω/
sq。
In step sl, as selection TiO2It, can be by sol gel process and using containing Ti's when colloidal sol is as crackle liquid
Prepared by raw material, wherein the raw material containing Ti can be butyl titanate, isopropyl titanate etc., and other raw material are diethanol
Amine, ethyl alcohol, deionized water,
Specific preparation process is as follows:
S11, a certain proportion of diethanol amine and dehydrated alcohol are mixed, butyl titanate is slowly dropped into shape after mixing
At solution A；
S12, deionized water and dehydrated alcohol are mixed to form B solution；
S13, respectively by A, B solution utilize magnetic stirrer；
S14, B solution is slowly added to be stirred in A, ultimately forms colloidal sol；
In step s11, isopropyl titanate is also can be selected in the titanium source；
Wherein, Ti (OC4H9)4With H2The molar ratio of O is 0.25-4, wherein Ti (OC4H9)4Substance amount be 0.5-
2mol, H2The amount of the substance of O is 0.5-2mol；
C2H5The molar ratio of OH and DEA is 6.6-60, wherein C2H5The amount of the substance of OH is 20-30mol, the substance of DEA
Amount is 20-30mol.
In step s12, step s13, mixing time is 1-3h.
Embodiment 1
In the present embodiment, 50 μ are taken as crackle liquid using untreated water soluble acrylic resin CA-600 lotion
Its spin coating is set spin coating parameters as even painting revolving speed by L acrylic resin CA-600 lotion on the glass substrate, in spin coating process
500rpm, even painting time 15s, spin coating revolving speed are 1000-5000rpm, spin-coating time 20s, are heated up with the heating rate of 200 DEG C/h
1h is kept the temperature at a temperature of 200 DEG C afterwards, obtains the cracked plate pattern under the conditions of different rotating speeds as shown in Figure 1, from the difference in Fig. 1
In the cracked plate pattern that crackle liquid under speed conditions is formed it can be seen that with spin coating revolving speed increase, the line width of cracked plate
It gradually becomes smaller, mesh quantity is more and more finer and close.In Fig. 1, when spin coating revolving speed is 5000rpm, template thickness is about 4 μm.
40 μ L are coated on cracked plate without the same spin coating proceeding of particle silver ink water, in 200 DEG C of temperature 1h, with
Furnace is cooled to room temperature, and observes that the surface topography of crackle and the existence without particle silver ink water and sectional view are as shown in Figure 2.
Entire sample is placed in supersonic cleaning machine again therewith and carries out ultrasonic cleaning 3min, removes acrylic resin CA-600
Cracked plate, the cleaning agent in supersonic cleaning machine use ratio for the mixed solution of the dehydrated alcohol of 2:1 and deionized water, final
To electrically conducting transparent silver grid film, as shown in Figure 3.
Fig. 4 then indicates that the transmissivity of the cracked plate electrically conducting transparent silver grid film obtained under the conditions of different rotating speeds is bent
Line.Wherein, when spin coating revolving speed is 1000rpm, transmitance reaches 82.7%, and film rectangular resistance is 32.9 Ω/sq；Spin coating revolving speed
When being 2000rpm, transmitance is 81.5%, and film rectangular resistance is 10.6 Ω/sq；When spin coating revolving speed is 3000rpm, transmitance
It is 75.4%, film rectangular resistance is 9.6 Ω/sq；When spin coating revolving speed is 4000rpm, transmitance is 71.2%, the square of film
Resistance is 1.2 Ω/sq.
Embodiment 2
In the present embodiment, water soluble acrylic resin's CA-600 lotion system of 20 μ L, 40 μ L, 70 μ L, 80 μ L are taken respectively
Make cracked plate, in manufacturing process with the revolving speed of 5000rpm by the spin coating of crackle liquid on the glass substrate, spin-coating time 20s, with
The heating rate of 200 DEG C/h dry 1h at a temperature of final 250 DEG C observes that the cracked plate of different-thickness as shown in Figure 5 is cut
Face figure, wherein the thickness of crackle template distinguishes 18 μm, 7 μm, 5 μm, 3 μm.As can be drawn from Figure 5: passing through control water solubility third
The coated weight of olefin(e) acid resin CA-600 emulsion template can control the thickness of template, and then control electrically conducting transparent silver obtained
The thickness of network film.
Embodiment 3
In the present embodiment, using TiO2Colloidal sol is as crackle liquid.TiO2Crack morphology figure such as Fig. 6 institute of colloidal sol cracked plate
Show.In preparation TiO2When colloidal sol crackle liquid, raw material of the butyl titanate as titanium are selected, glacial acetic acid is substituted using diethanol amine
As complexing agent, stable flaxen TiO 2 sol is prepared at normal temperature.
Prepare TiO2When colloidal sol, Ti (OC4H)4、C2H5OH、DEA、H2The molar ratio of O is 1:25:1:1, works as TiO2Colloidal sol is split
Line drop dosage is 30 μ L, and heating temperature is 150 DEG C, keeps the temperature 30min, is slowly dropped to room temperature, can promote the cracking of crackle liquid.
As Ti (OC4H)4With H2When the molar ratio of O is 1:1.5, the crackle of generation is most carefully 0.593 μm.
TiO by no particle silver ink water with the revolving speed spin coating of 3000rpm on the glass substrate2On colloidal sol cracked plate, by it
It places and is heated up in a vacuum drying oven with the heating rate of 200 DEG C/h, keep the temperature half an hour under the conditions of 250 DEG C, cool to the furnace
Room temperature finally places it in the ultrasonic cleaning agent equipped with dehydrated alcohol and is cleaned by ultrasonic 5min, removes TiO2Colloidal sol cracked plate,
Obtain electrically conducting transparent silver grid film.
Fig. 7 is different TiO2The transmittance curve comparison diagram of electrically conducting transparent silver grid film obtained under colloidal sol density,
The template prepared under 1000rpm and 3000rpm spin coating revolving speed has respectively obtained low-density grid film and higher-density
Silver-colored grid transparent conductive film, when spin coating revolving speed is 1000rpm, transmitance reaches 60.7%, film rectangular resistance be 28 Ω/
sq；When spin coating revolving speed is 3000rpm, transmitance is 92.1%, and film rectangular resistance is 50 Ω/sq.
Grid interconnected in the present invention in substrate will not mutually " bridging ", and regular metal grill can be ideally
The dense distribution of seepage flow, the contact resistance at grid knot and conducting wire between elimination conducting wire, network have lesser curvature
Radius meets the requirement of flexibility, has preferable flexibility as the flexible transparent conductive film of representative using metal grill and leads
Electrically, it is amenable to repeatedly bend and bend, can form a film at room temperature.The preparation side of electrically conducting transparent silver grid film in the present invention
Method is at low cost and does not need precision instrument, and the method for manufacturing thin film in the present invention easily can be used to synthesize required colloidal sol mould
Plate, and acrylic resin CA-600 lotion can directly be bought.
The present invention prepares the technique of electrically conducting transparent silver grid thin-film material, is made with the material easy to crack of mentioned above two kinds
For template, the film of a variety of silver-colored grid patterns can be provided in conjunction with the setting of spin coating proceeding parameter, and then obtains different transmitances
With the transparent conductive film of different square resistances.The present invention facilitates the upgrading innovation for meeting transparent conductive film field, for not
Carry out intelligent wearable instrument and equipment and carrier is provided.
It is to be appreciated that describing the skill simply to illustrate that of the invention to what specific embodiments of the present invention carried out above
Art route and feature, its object is to allow those skilled in the art to can understand the content of the present invention and implement it accordingly, but
The present invention is not limited to above-mentioned particular implementations.All various changes made within the scope of the claims are repaired
Decorations, should be covered by the scope of protection of the present invention.
Claims (10)
1. a kind of electrically conducting transparent silver grid film, it is characterised in that:
The electrically conducting transparent grid film is prepared by no particle silver ink water, is prolonged including what is be made by silver-colored grid lines in in-plane
The irregular grid of exhibition, the grid constitute conduction region and insulation layer, and the conduction region is that the shape that silver-colored grid lines is made into is not advised
Grid frame then, the insulation layer are the white space that silver-colored grid lines impales.
2. electrically conducting transparent silver grid film according to claim 1, it is characterised in that:
The electrically conducting transparent silver grid film film thickness is 2-20 μm, and transmitance is 60~92%, and square resistance is 1-50 Ω/sq.
3. a kind of electrically conducting transparent silver grid method for manufacturing thin film, it is characterised in that:
The preparation method the following steps are included:
S1: it coats in crackle plate surface without particle silver ink water, is dried, obtains silver-colored grid film；
S2: the silver-colored grid film that step S1 is obtained is cleaned by ultrasonic, and finally obtains electrically conducting transparent silver grid film.
4. the preparation method of electrically conducting transparent silver grid film according to claim 3, it is characterised in that:
The cracked plate is coated in substrate surface by crackle liquid, is made after being dried；
The crackle liquid is selected from water soluble acrylic resin CA-600 lotion, TiO2Colloidal sol, SiO2Colloidal sol, crackle nail polish, egg white
And any one of ice template.
5. the preparation method of electrically conducting transparent silver grid film according to claim 4, it is characterised in that:
TiO2Sol preparation step is as follows:
S11, diethanol amine and dehydrated alcohol are mixed, is slowly dropped into butyl titanate to form solution A after mixing；
S12, deionized water and dehydrated alcohol are mixed to form B solution；
S13, respectively by A, B solution utilize magnetic stirrer 1-3h；
S14, B solution is slowly added to be stirred for 1-3h in A, ultimately forms colloidal sol；
Wherein, Ti (OC4H9)4With H2The molar ratio of O is 0.25-4；
C2H5The molar ratio of OH and DEA is 6.6-60.
6. the preparation method of electrically conducting transparent silver grid film according to claim 4 or 5, it is characterised in that:
The substrate is selected from glass, polyethylene terephthalate, polyimides, dimethyl silicone polymer and phase paper base plate
Any one of.
7. the preparation method of electrically conducting transparent silver grid film according to claim 3 or 4, it is characterised in that:
The crackle liquid the coating method of substrate surface, the no particle silver ink water the crackle plate surface coating method
It is spin coating, spin coating parameters are even painting revolving speed 500rpm in the spin coating process, and even painting time 15s, spin coating revolving speed is 1000-
5000rpm, spin-coating time 20s.
8. the preparation method of electrically conducting transparent silver grid film according to claim 3 or 4, it is characterised in that:
The crackle liquid the coating method of substrate surface, the no particle silver ink water the crackle plate surface coating method
For drop coating, spraying, blade coating or magnetron sputtering.
9. the preparation method of electrically conducting transparent silver grid film according to claim 7 or 8, it is characterised in that:
The drying process of the crackle liquid and the no particle silver ink water is using heating plate or vacuum oven, and heating rate is set
For 40-200 DEG C/h, drying temperature is set as 100-250 DEG C, soaking time 0.5-2h, after with furnace be down to room temperature.
10. the preparation method of electrically conducting transparent silver grid film according to claim 7 or 8, it is characterised in that: step S2
In,
The ultrasonic cleaning agent is dehydrated alcohol, dehydrated alcohol and deionized water mixed solution, and the ultrasonic cleaning time is set as 3-
10min。
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| CN110600165A (en) * | 2019-08-24 | 2019-12-20 | 泉州柔丝蓝新材料科技有限公司 | Flexible transparent conductive film and preparation process thereof |
| CN110600165B (en) * | 2019-08-24 | 2023-12-08 | 厦门派恩杰科技有限公司 | Flexible transparent conductive film and preparation process thereof |
| CN110965098A (en) * | 2019-11-30 | 2020-04-07 | 华南理工大学 | Porous multi-stage structure anodic aluminum oxide template and preparation method thereof |
| CN110838386A (en) * | 2019-12-13 | 2020-02-25 | 哈尔滨工业大学 | Shape memory embedded double-layer metal grid conductive film and preparation method thereof |
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