CN109634020A - Based on nano-cellulose-silver nanowires electroluminescent device and its application - Google Patents
Based on nano-cellulose-silver nanowires electroluminescent device and its application Download PDFInfo
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- CN109634020A CN109634020A CN201811589373.1A CN201811589373A CN109634020A CN 109634020 A CN109634020 A CN 109634020A CN 201811589373 A CN201811589373 A CN 201811589373A CN 109634020 A CN109634020 A CN 109634020A
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
- G02F1/153—Constructional details
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
Abstract
The invention discloses a kind of based on nano-cellulose-silver nanowires electroluminescent device, is prepared by following steps: a, using dimethyl silicone polymer as raw material, prepares polydimethylsiloxanefilm film；B, using polydimethylsiloxanefilm film as raw material, hydrophily polydimethylsiloxanefilm film is prepared；C, using dimethyl silicone polymer, luminescent powder, barium titanate as raw material, luminescent layer solution is prepared；D, using bleached wood pulp fiber as raw material, nano-cellulose suspension is prepared；E, the mixed liquor of nano-cellulose suspension Yu aqueous silver nanowires dispersion liquid is prepared；F, mixed liquor is sprayed on hydrophily polydimethylsiloxanefilm film surface, spin coating luminescent layer solution, one layer of electrode of top laminate to get.Electroluminescent device electric conductivity provided by the invention is highly stable, and light emission luminance strong to the adhesiveness of substrate is stablized.
Description
Technical field
The invention belongs to macromolecule photoelectric Material Fields, and in particular to a kind of based on nano-cellulose-silver nanowires electricity
Electroluminescence device and its application.
Background technique
Dimethyl silicone polymer (Polydimethylsiloxane, PDMS) due to good optics, tensility,
Viscoplasticity, mechanical stability, translucency, easily molded, biocompatibility and chemical property and process are simple, cheap etc.
Advantage is widely used in flexible electronic research field.But the high hydrophobicity of dimethyl silicone polymer is simultaneously handled in surface hydrophilic
After be easy to happen it is hydrophobic recovery and to large biological molecule have stronger adsorption characteristic, limit its application range.
Silver nanowires has the high grade of transparency and electric conductivity, and intrinsic good mechanical strength is excellent with inexpensive production technology
Point.Silver nanowires film can effectively adapt to strain by orienting silver nanowires along draw direction, while answer > 20%
Become the lower excellent electric contact kept between silver nanowires.Highly stretchable conductor passes through being deposited on by means of buckling strategy
Silver nanowires manufacture on elastic base plate.Silver nanowires composite conductor has now been developed, realizes the low thin layer of 10-33ohm/sq
Resistance, the high-transmission rate of 82-94% and the draftability of 40-460%.The ultimate challenge that nano wire laminated film faces is by line-
Contact resistance caused by line connects, this can be welded by plasma and the technologies such as chemistry welding solve, these technologies will be received
Rice noodles knot links together and reduces contact resistance.They are widely studied in flexible El element, exhibit improvements over thin
The advantage of film counterpart.But need a kind of cost-effective solution still to overcome complicated patterning, transfer and viscous
Conjunction process.
Cellulose nanocrystal body (CNCs) derived from natural is emerging nano material, shows high intensity, high surface
Long-pending and adjustable surface chemistry, permission and polymer, nano particle, the controlled interaction of small molecule and biomaterial.CNC
Ⅱs
Then sulphuric acid hydrolysis is extracted from native cellulose source such as wood pulp or cotton for first sodium hydroxide alkali cleaning, on the surface
Leave negatively charged sulfate hemiester group.The hydrolytic process preferentially cracks the cellulose fibre in amorphous domain, makes height
The section of crystallization keeps complete.Nano-cellulose fiber (CNC II) length is 46 ± 18nm, and cross sectional dimensions only has 5 ± 1nm.
These high aspect ratio nano particles show impressive mechanical performance and adjustable surface chemical property.They
High surface-to-volume ratio can enhance and polymer, and the interaction of other nano particles and small molecule is simultaneously in combination.
Transparent and stretchable electricity is manufactured by the way that silver nanowires network thin-film to be embedded in or be sprayed in Stretchable polymeric
Pole.In view of the property of polymer, such as glass transition temperature, draftability, the transparent and binding force with network to be transferred.
If the bonding interaction between polymer and conductive network is weak, insufficient transfer will lead to aobvious in thin, transparent layer
Electric conductivity reduce.Instead of using insertion and transfer method, silver nanowires network is sprayed directly into elastic substrates, is utilized
This method, can be to avoid the damage in transfer process to conduction percolation network, to keep high conductivity in hyaline layer.
But due to adhesiveness weak between silver nanowires and dimethyl silicone polymer surface so that conductive layer it is highly unstable with it is uneven.
Soft electronic equipment is becoming the new technology of the boundary and limitation that push conventional planar and rigid device.Deformable electricity
Photoluminescence (EL) device brings special interest, because they are expected to the Monitor-centric' for anticipation in the near future
Bring a possibility that a large amount of new in the world.By integrating luminescent layer array with diaphragm pressure sensor, a kind of user's friendship is illustrated
Mutual formula electronic skin can show directly and quantitatively the pressure applied in equipment, so that emissive porwer changes, this will provide and applies
Stressed instant quantization visualization.User interactive system will be in automobile control panel, interaction type input apparatus, robot and strong
Interesting application is found in health monitoring device.The challenge of deformable electroluminescent (EL) device first is that they in a stretched state
The device stability of significant impact.It is necessary to have the stabilization conductors of satisfactory electrical conductivity and the transparency in order to overcome the problem.
Currently on the market there are no having preferable aqueous silver nanowires solution, can be painted on by hydrophily
The dimethyl silicone polymer surface of reason obtains uniform and stable conductive film, provides for stretchable electroluminescent device uniform and stable
Electrode.
Summary of the invention
It is a kind of based on nano-cellulose-silver nanowires electricity in order to overcome the deficiencies in the prior art, the present invention provides
Electroluminescence device and its application.
In order to solve the above-mentioned technical problem, the present invention adopts the following technical scheme:
It is a kind of based on nano-cellulose-silver nanowires electroluminescent device, be prepared by following steps:
A, using dimethyl silicone polymer as raw material, polydimethylsiloxanefilm film is prepared；
B, using polydimethylsiloxanefilm film as raw material, hydrophily polydimethylsiloxanefilm film is prepared；
C, using dimethyl silicone polymer, luminescent powder, barium titanate as raw material, luminescent layer solution is prepared；
D, using bleached wood pulp fiber as raw material, nano-cellulose suspension is prepared；
E., the mixed liquor of nano-cellulose suspension Yu aqueous silver nanowires dispersion liquid is prepared；
F., the obtained mixed liquor of step e is sprayed on hydrophily polydimethylsiloxanefilm film surface made from step b,
Luminescent layer solution made from spin-coating step c, in one layer of electrode of top laminate to get based on nano-cellulose-silver nanowires electricity
Electroluminescence device.
Preferably, in step a polydimethylsiloxanefilm film preparation method the following steps are included: (1) weigh 1~
10g dimethyl silicone polymer solution is added the curing agent of 0.1~1g, said mixture is sufficiently stirred using magnetic stirring apparatus.Claim
1~10g mixing drop-coated levelling on the glass sheet is taken, solidifies 30~120min in 40~80 DEG C of baking oven, from sheet glass
Removing；Another polydimethylsiloxanefilm film is prepared with same method.
Preferably, in step b hydrophily polydimethylsiloxanefilm film preparation method the following steps are included:
(1) by polydimethylsiloxanefilm film be placed in hydrochloric acid and hydrogen peroxide composition oxidation solution impregnate in 5~
30min aoxidizes solution H2O, HCl and H2O2It is mixed with the volume ratio of 2:1:1~10:1:1, aoxidizes polydimethylsiloxanes
Then alkane film surface rinses 1~10min with deionized water, then rinses 1~10min, nitrogen drying with ethyl alcohol；
(2) by polydimethylsiloxanefilm film be put into the mixed solution with second alcohol and water be added APTES after reaction 30~
60min, the volume ratio of second alcohol and water is 10:1~25:1 in mixed solution, and APTES accounts for the hundred of the gross mass of ethyl alcohol and aqueous solution
Divide than being 2~10%, is dried through nitrogen；
(3) 8~15mM Tris buffer solution is prepared using distilled water, and pH is maintained 8~8.5 by the way that HCl is added,
Polydimethylsiloxanefilm film is put into containing 1~5mg mL-1In the solution of dopamine hydrochloride stirring 12~for 24 hours after, use
Distilled water cleaning is dried through nitrogen, obtains hydrophily polydimethylsiloxanefilm film.
Preferably, in step c luminescent layer solution preparation method the following steps are included:
(1) weigh 1~10g dimethyl silicone polymer solution, be added 0.1~1g curing agent, 2~20g luminescent powder, 0.5~
Said mixture is sufficiently stirred using magnetic stirring apparatus in 5g barium titanate, places it in static 20~60min in vacuum drying oven.
Preferably, in step d nano-cellulose suspension preparation method the following steps are included:
(1) NaOH for weighing 25.45~101.78g is added in the stirring distilled water of 100~400mL, complete to NaOH
After dissolution, the bleached wood pulp cellulose powder that 5~20g is crushed is added into reaction system, filtering after 2~8h of reaction to pH is 8
~8.5；
(2) 60~65% H of 50~200g is configured2SO4Solution；
(3) oil bath is warming up to 44-45 DEG C, by configured H2SO4Solution is put into oil bath, to H2SO4Solution and oil
Bath temperature is consistent, to H2SO4It is slowly added to the wood pulp cellulose powder handled by NaOH in solution, is stirred always using agitating paddle
Water is added to terminate reaction after mixing 30~120min；
(4) cellulose that is acid hydrolysis for terminating reaction is poured into beaker, after distilled water quiescent settling is added several times, is fallen
Enter in bag filter, dialysis to neutrality is taken out；
(5) in ice-water bath, ultrasound 30-60min removes acidolysis cellulose under 200~400W power receives for cellulose
It is spare to be placed on stored under refrigeration in refrigerator, that is, prepares nanofibers by rice fiber for the fiber nanofiber suspension being prepared
Plain suspension.
Preferably, the preparation method of the mixed liquor of nano-cellulose suspension and silver nanowires solution includes in step e
Following steps:
(1) by 1~10mg mL-1Silver nanowires solution adds distilled water to be diluted to 0.2~1.5mg mL-1Silver nanowires is molten
Liquid；
(2) it weighs nano-cellulose suspension and 0.2~1.5mg mL is added-1Silver nanowires solution, nano-cellulose add
Enter 5~35wt% that amount is silver nanowires solid content, at room temperature 30~120min of magnetic agitation, to form uniform and stable lead
Electric compound suspension.
Preferably, nano-cellulose-silver nanowires combination electrode prepares the system of stretchable electroluminescent device in step f
Preparation Method the following steps are included:
(1) draw 0.5~2.5ml electrically conductive composite suspension spray be placed on it is hydrophilic on 40~60 DEG C of warm tables
Property polydimethylsiloxanefilm film on, obtain bottom composite conductive layers, similarly, preparation top composite conductive layers；
(2) luminescent layer solution is spin-coated on the composite conductive layers of bottom, is placed on 5~10min in 40~80 DEG C of baking ovens；
(3) by top composite conductive layers lamination on the light-emitting layer, bottom, top composite conductive layers access copper strips to get
To stretchable electroluminescent device.
A kind of application based on nano-cellulose-silver nanowires electroluminescent device will be based on made from the above method
Nano-cellulose-silver nanowires electroluminescent device applications are in flexible display screen or luminous electron skin.
The beneficial effects of the present invention are:
The present invention is thin in hydrophily dimethyl silicone polymer using direct spraying nano-cellulose-silver nanowires combination electrode
Film surface, spin coating luminescent layer are laminated top electrodes on the light-emitting layer and prepare stretchable electroluminescent device in bottom electrode.
1, aqueous silver nanowires dispersion liquid is easy to oxidize, needs to use within the regular hour, which has limited aqueous silver to receive
The use of rice noodles.Using the reproducible nano-cellulose of green as dispersing agent and antioxidant, sufficiently solves aqueous silver and receive
The problem of oxidation of rice noodles, the roughness for reducing fine silver nano wire conductive film, and improve its dispersibility.
2, it is inspired by biological mussel, the poly-dopamine layer obtained by dopamine oxidation polymerization has stronger adhesive force.
Aqueous silver nanowires dispersion liquid is sprayed on the dimethyl silicone polymer surface through dopamine hydrophilic treated, due to the mistake of moisture
It goes, conductive network can not form a film, very poor with the adhesiveness of substrate.By the way that the reproducible cellulose nano-fibrous suspension of green is added
Liquid is sprayed on hydrophilic through dopamine by the composite conducting suspension that its intrinsic aqueous phase dispersibility is uniformly mixed
On the dimethyl silicone polymer surface of processing, nano-cellulose-silver nanowires composite conductive film is obtained, stable conductive mesh is formed
Network and its with the preferable adhesiveness in base.
3, composite conducting suspension is painted on the dimethyl silicone polymer surface through dopamine hydrophilic treated, can be with
The damage of silver nanowires conductive network caused by transfer method is embedded in about silver nanowires before instead and silver nanowires is adhered to
It is not transferred on flexible polymer in substrate of glass, reduces its electric conductivity and causes the waste of raw material.
4, hydrophilic treated is carried out to dimethyl silicone polymer, the manufacturing process of direct spraying is that realization is stretchable/wearable
The feasible solution of the extensive and low-cost construction of electronics.
Detailed description of the invention
Fig. 1 is the resulting nano-cellulose of embodiment 2-silver nanowires composite conductive film scanning electron microscope (SEM) photograph；
Fig. 2 is the resulting nano-cellulose of embodiment 2-silver nanowires composite conductive film atomic force microscopy diagram；
Fig. 3 is nano-cellulose-silver nanowires composite conductive film light transmittance obtained by different nanofiber cellulose contents and side
Resistance figure；
Fig. 4 is the resulting nano-cellulose of embodiment 2-silver nanowires composite conductive film and the Yin Na that nano-cellulose is not added
The time of rice noodles conductive film and the curve graph of sheet resistance；
Fig. 5 is that the resulting nano-cellulose of embodiment 2-silver nanowires mixed liquor is sprayed on hydrophily dimethyl silicone polymer
In substrate and adhesiveness of the silver nanowires solution spraying of nano-cellulose in hydrophily dimethyl silicone polymer substrate is not added
Curve graph；
Fig. 6 is the stretchable electroluminescent device of the resulting composite conducting film layer of embodiment 2 preparation under different conditions
Brightness variation curve figure and pictorial diagram.
Specific embodiment
Present invention will be further described below with reference to the accompanying drawings and specific embodiments:
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within protection scope of the present invention.In embodiment
Silver nanowires is the finished product bought from market.
Embodiment 1:
Step 1, the preparation of polydimethylsiloxanefilm film, specific method step include:
(1) 1g dimethyl silicone polymer solution is weighed, the curing agent of 0.1g is added, is sufficiently stirred using magnetic stirring apparatus
State mixture.1.1g mixing drop-coated levelling on the glass sheet is weighed, solidifies 2h in 80 DEG C of baking oven, is shelled from sheet glass
From；Similarly, another polydimethylsiloxanefilm film is prepared.
Step 2, the preparation of hydrophily polydimethylsiloxanefilm film, specific method step include:
(1) polydimethylsiloxanefilm film is placed in and uses H2O, HCl and H2O2The oxygen being mixed with the volume ratio of 2:1:1
Change solution and impregnate 5min reaction, aoxidizes polydimethylsiloxanefilm film surface, then rinse 1min with deionized water, then use ethyl alcohol
Rinse 1min, nitrogen drying；(2) polydimethylsiloxanefilm film is put into second alcohol and water to be added in the mixed solution of 10:1
30min is reacted after the APTES of 2wt%, is dried through nitrogen；(3) 8mM Tris buffer solution is prepared using distilled water, and by adding
Enter HCl and pH is maintained~8.5, polydimethylsiloxanefilm film is put into containing 1mg mL-1In the solution of dopamine hydrochloride
It after stirring for 24 hours, is dried wash with distilled water through nitrogen, obtains hydrophily polydimethylsiloxanefilm film.
Step 3, the preparation of luminescent layer solution, specific method step include:
(1) 1g dimethyl silicone polymer solution is weighed, 0.1g curing agent, 2g luminescent powder, 0.5g barium titanate is added, utilizes magnetic
Said mixture is sufficiently stirred in power blender, places it in static 20min in vacuum drying oven.
Step 4, the preparation of nano-cellulose suspension, specific method step include:
(1) NaOH for weighing 25.45g is added in the stirring distilled water of 100mL, after NaOH is completely dissolved, Xiang Fanying
The bleached wood pulp cellulose powder that 5g is crushed is added in system, filters after reacting 2h to the close neutrality of pH；(2) configure 50g's
60% H2SO4Solution；(3) oil bath is warming up to 44-45 DEG C, by configured H2SO4Solution is put into oil bath, to H2SO4
Solution is consistent with oil bath temperature.To H2SO4It is slowly added to the wood pulp cellulose powder handled by NaOH in solution, utilizes stirring
Paddle adds water to terminate reaction after stirring 1h always；(4) cellulose that is acid hydrolysis for terminating reaction is poured into beaker, it is quiet that distilled water is added
It after only settling several times, is poured into bag filter, dialysis to neutrality is taken out；(5) ultrasonic under 300W power in ice-water bath
30-60min removes acidolysis cellulose to be cellulose nano-fibrous, and the cellulose nano-fibrous suspension being prepared is placed on
Stored under refrigeration is spare in refrigerator, that is, prepares nano-cellulose suspension.
Step 5, the preparation of nano-cellulose-silver nanowires suspension is mixed, specific method step includes:
(1) by 1mg mL-1Silver nanowires solution adds distilled water to be diluted to 0.2mg mL-1Silver nanowires solution；At room temperature
Magnetic agitation 1h, to form uniform and stable electrically conductive composite suspension.
Step 6, nano-cellulose-silver nanowires combination electrode prepares the preparation of stretchable electroluminescent device, specific
Method and step includes:
(1) the electrically conductive composite suspension spray of 0.5ml is drawn in hydrophilic poly- two be placed on 60 DEG C of warm tables
On methylsiloxane film, bottom composite conductive layers are obtained, similarly, preparation top composite conductive layers；(2) luminescent layer solution is revolved
It is coated on the composite conductive layers of bottom, is placed on 5min in 80 DEG C of baking ovens；(3) on the light-emitting layer by the lamination of top composite conductive layers,
Copper strips is accessed in bottom, top composite conductive layers to get stretchable electroluminescent device is arrived.
Embodiment 2:
Step 1, the preparation of polydimethylsiloxanefilm film, specific method step include:
(1) 2g dimethyl silicone polymer solution is weighed, the curing agent of 0.2g is added, is sufficiently stirred using magnetic stirring apparatus
State mixture.1.1g mixing drop-coated levelling on the glass sheet is weighed, solidifies 2h in 80 DEG C of baking oven, is shelled from sheet glass
From；Similarly, another polydimethylsiloxanefilm film is prepared.
Step 2, the preparation of hydrophily polydimethylsiloxanefilm film, specific method step include:
(1) polydimethylsiloxanefilm film is placed in and uses H2O, HCl and H2O2The oxygen being mixed with the volume ratio of 5:1:1
Change solution and impregnate 5min reaction, aoxidizes polydimethylsiloxanefilm film surface, then rinse 10min with deionized water, then use second
Alcohol rinses 5min, nitrogen drying；(2) polydimethylsiloxanefilm film is put into second alcohol and water to add in the mixed solution of 19:1
30min is reacted after entering the APTES of 2wt%, is dried through nitrogen；(3) 10mM Tris buffer solution is prepared using distilled water, and led to
It crosses addition HCl and pH is maintained~8.5, polydimethylsiloxanefilm film is put into containing 1mg mL-1Dopamine hydrochloride it is molten
It after being stirred for 24 hours in liquid, is dried wash with distilled water through nitrogen, obtains hydrophily polydimethylsiloxanefilm film.
Step 3, the preparation of luminescent layer solution, specific method step include:
(1) 1g dimethyl silicone polymer solution is weighed, 0.1g curing agent, 2g luminescent powder, 0.5g barium titanate is added, utilizes magnetic
Said mixture is sufficiently stirred in power blender, places it in static 20min in vacuum drying oven.
Step 4, the preparation of nano-cellulose suspension, specific method step include:
(1) NaOH for weighing 50.89g is added in the stirring distilled water of 200mL, after NaOH is completely dissolved, Xiang Fanying
The bleached wood pulp cellulose powder that 10g is crushed is added in system, filters after reacting 4h to the close neutrality of pH；(2) configure 200g's
64% H2SO4Solution；(3) oil bath is warming up to 44-45 DEG C, by configured H2SO4Solution is put into oil bath, to H2SO4
Solution is consistent with oil bath temperature.To H2SO4It is slowly added to the wood pulp cellulose powder handled by NaOH in solution, utilizes stirring
Paddle adds water to terminate reaction after stirring 1h always；(4) cellulose that is acid hydrolysis for terminating reaction is poured into the beaker of 1000mL, is added
Distilled water quiescent settling several times after, be poured into bag filter, dialysis to neutrality take out；(5) in ice-water bath, in 300W power
Acidolysis cellulose is removed the cellulose nano-fibrous suspension that be cellulose nano-fibrous, will be prepared by lower ultrasound 30-60min
It is spare that liquid is placed on stored under refrigeration in refrigerator, that is, prepares nano-cellulose suspension.
Step 5, the preparation of nano-cellulose-silver nanowires suspension is mixed, specific method step includes:
(1) by 10mg mL-1Silver nanowires solution adds distilled water to be diluted to 1mg mL-1Silver nanowires solution；(2) it takes certain
1mg mL is added in the 5wt% that the nano-cellulose suspension of amount accounts for silver nanowires solid content-1Silver nanowires solution, at room temperature magnetic
Power stirs 1h, to form uniform and stable electrically conductive composite suspension.
Step 6, nano-cellulose-silver nanowires combination electrode prepares the preparation of stretchable electroluminescent device, specific
Method and step includes:
(1) the electrically conductive composite suspension spray of 0.8ml is drawn in hydrophilic poly- two be placed on 60 DEG C of warm tables
On methylsiloxane film, bottom composite conductive layers are obtained, similarly, preparation top composite conductive layers；(2) luminescent layer solution is revolved
It is coated on the composite conductive layers of bottom, is placed on 5min in 80 DEG C of baking ovens；(3) on the light-emitting layer by the lamination of top composite conductive layers,
Copper strips is accessed in bottom, top composite conductive layers to get stretchable electroluminescent device is arrived.
Embodiment 3:
Step 1, the preparation of polydimethylsiloxanefilm film, specific method step include:
(1) 2g dimethyl silicone polymer solution is weighed, the curing agent of 0.2g is added, is sufficiently stirred using magnetic stirring apparatus
State mixture.1.1g mixing drop-coated levelling on the glass sheet is weighed, solidifies 2h in 80 DEG C of baking oven, is shelled from sheet glass
From；Similarly, another polydimethylsiloxanefilm film is prepared.
Step 2, the preparation of hydrophily polydimethylsiloxanefilm film, specific method step include:
(1) polydimethylsiloxanefilm film is placed in and uses H2O, HCl and H2O2The oxygen being mixed with the volume ratio of 5:1:1
Change solution and impregnate 5min reaction, aoxidizes polydimethylsiloxanefilm film surface, then rinse 10min with deionized water, then use second
Alcohol rinses 5min, nitrogen drying；(2) polydimethylsiloxanefilm film is put into second alcohol and water to add in the mixed solution of 19:1
30min is reacted after entering 2%APTES, is dried through nitrogen；(3) 10mM Tris buffer solution is prepared using distilled water, and by adding
Enter HCl and pH is maintained~8.5, polydimethylsiloxanefilm film is put into containing 1mg mL-1In the solution of dopamine hydrochloride
It after stirring for 24 hours, is dried wash with distilled water through nitrogen, obtains hydrophily polydimethylsiloxanefilm film.
Step 3, the preparation of luminescent layer solution, specific method step include:
(1) 1g dimethyl silicone polymer solution is weighed, 0.1g curing agent, 2g luminescent powder, 0.5g barium titanate is added, utilizes magnetic
Said mixture is sufficiently stirred in power blender, places it in static 20min in vacuum drying oven.
Step 4, the preparation of nano-cellulose suspension, specific method step include:
(1) NaOH for weighing 50.89g is added in the stirring distilled water of 200mL, after NaOH is completely dissolved, Xiang Fanying
The bleached wood pulp cellulose powder that 10g is crushed is added in system, filters after reacting 4h to the close neutrality of pH；(2) configure 200g's
64% H2SO4Solution；(3) oil bath is warming up to 44-45 DEG C, by configured H2SO4Solution is put into oil bath, to H2SO4
Solution is consistent with oil bath temperature.To H2SO4It is slowly added to the wood pulp cellulose powder handled by NaOH in solution, utilizes stirring
Paddle adds water to terminate reaction after stirring 1h always；(4) cellulose that is acid hydrolysis for terminating reaction is poured into the beaker of 1000mL, is added
Distilled water quiescent settling several times after, be poured into bag filter, dialysis to neutrality take out；(5) in ice-water bath, in 300W power
Acidolysis cellulose is removed the cellulose nano-fibrous suspension that be cellulose nano-fibrous, will be prepared by lower ultrasound 30-60min
It is spare that liquid is placed on stored under refrigeration in refrigerator, that is, prepares nano-cellulose suspension.
Step 5, the preparation of nano-cellulose-silver nanowires suspension is mixed, specific method step includes:
(1) by 10mg mL-1Silver nanowires solution adds distilled water to be diluted to 1mg mL-1Silver nanowires solution；(2) it takes certain
1mg mL is added in the 15wt% that the nano-cellulose suspension of amount accounts for silver nanowires solid content-1Silver nanowires solution, at room temperature
Magnetic agitation 1h, to form uniform and stable electrically conductive composite suspension.
Step 6, nano-cellulose-silver nanowires combination electrode prepares the preparation of stretchable electroluminescent device, specific
Method and step includes:
(1) the electrically conductive composite suspension spray of 0.8ml is drawn in hydrophilic poly- two be placed on 60 DEG C of warm tables
On methylsiloxane film, bottom composite conductive layers are obtained, similarly, preparation top composite conductive layers；(2) luminescent layer solution is revolved
It is coated on the composite conductive layers of bottom, is placed on 5min in 80 DEG C of baking ovens；(3) on the light-emitting layer by the lamination of top composite conductive layers,
Copper strips is accessed in bottom, top composite conductive layers to get stretchable electroluminescent device is arrived.
Embodiment 4:
Step 1, the preparation of polydimethylsiloxanefilm film, specific method step include:
(1) 2g dimethyl silicone polymer solution is weighed, the curing agent of 0.2g is added, is sufficiently stirred using magnetic stirring apparatus
State mixture.1.1g mixing drop-coated levelling on the glass sheet is weighed, solidifies 2h in 80 DEG C of baking oven, is shelled from sheet glass
From；Similarly, another polydimethylsiloxanefilm film is prepared.
Step 2, the preparation of hydrophily polydimethylsiloxanefilm film, specific method step include:
(1) polydimethylsiloxanefilm film is placed in and uses H2O, HCl and H2O2The oxygen being mixed with the volume ratio of 5:1:1
Change solution and impregnate 5min reaction, aoxidizes polydimethylsiloxanefilm film surface, then rinse 10min with deionized water, then use second
Alcohol rinses 5min, nitrogen drying；(2) polydimethylsiloxanefilm film is put into second alcohol and water to add in the mixed solution of 19:1
30min is reacted after entering 2%APTES, is dried through nitrogen；(3) 10mM Tris buffer solution is prepared using distilled water, and by adding
Enter HCl and pH is maintained~8.5, polydimethylsiloxanefilm film is put into containing 1mg mL-1In the solution of dopamine hydrochloride
It after stirring for 24 hours, is dried wash with distilled water through nitrogen, obtains hydrophily polydimethylsiloxanefilm film.
Step 3, the preparation of luminescent layer solution, specific method step include:
(1) 1g dimethyl silicone polymer solution is weighed, 0.1g curing agent, 2g luminescent powder, 0.5g barium titanate is added, utilizes magnetic
Said mixture is sufficiently stirred in power blender, places it in static 20min in vacuum drying oven.
Step 4, the preparation of nano-cellulose suspension, specific method step include:
(1) NaOH for weighing 50.89g is added in the stirring distilled water of 200mL, after NaOH is completely dissolved, Xiang Fanying
The bleached wood pulp cellulose powder that 10g is crushed is added in system, filters after reacting 4h to the close neutrality of pH；(2) configure 200g's
64% H2SO4Solution；(3) oil bath is warming up to 44-45 DEG C, by configured H2SO4Solution is put into oil bath, to H2SO4
Solution is consistent with oil bath temperature.To H2SO4It is slowly added to the wood pulp cellulose powder handled by NaOH in solution, utilizes stirring
Paddle adds water to terminate reaction after stirring 1h always；(4) cellulose that is acid hydrolysis for terminating reaction is poured into the beaker of 1000mL, is added
Distilled water quiescent settling several times after, be poured into bag filter, dialysis to neutrality take out；(5) in ice-water bath, in 300W power
Acidolysis cellulose is removed the cellulose nano-fibrous suspension that be cellulose nano-fibrous, will be prepared by lower ultrasound 30-60min
It is spare that liquid is placed on stored under refrigeration in refrigerator, that is, prepares nano-cellulose suspension.
Step 5, the preparation of nano-cellulose-silver nanowires suspension is mixed, specific method step includes:
(1) by 10mg mL-1Silver nanowires solution adds distilled water to be diluted to 1mg mL-1Silver nanowires solution；(2) it takes certain
1mg mL is added in the 25wt% that the nano-cellulose suspension of amount accounts for silver nanowires solid content-1Silver nanowires solution, at room temperature
Magnetic agitation 1h, to form uniform and stable electrically conductive composite suspension.
Step 6, nano-cellulose-silver nanowires combination electrode prepares the preparation of stretchable electroluminescent device, specific
Method and step includes:
(1) the electrically conductive composite suspension spray of 0.8ml is drawn in hydrophilic poly- two be placed on 60 DEG C of warm tables
On methylsiloxane film, bottom composite conductive layers are obtained, similarly, preparation top composite conductive layers；(2) luminescent layer solution is revolved
It is coated on the composite conductive layers of bottom, is placed on 5min in 80 DEG C of baking ovens；(3) on the light-emitting layer by the lamination of top composite conductive layers,
Copper strips is accessed in bottom, top composite conductive layers to get stretchable electroluminescent device is arrived.
Embodiment 5:
Step 1, the preparation of polydimethylsiloxanefilm film, specific method step include:
(1) 10g dimethyl silicone polymer solution is weighed, the curing agent of 1g is added, is sufficiently stirred using magnetic stirring apparatus
State mixture.5g mixing drop-coated levelling on the glass sheet is weighed, solidifies 2h in 80 DEG C of baking oven, is removed from sheet glass；
Similarly, another polydimethylsiloxanefilm film is prepared.
Step 2, the preparation of hydrophily polydimethylsiloxanefilm film, specific method step include:
(1) polydimethylsiloxanefilm film is placed in and uses H2O, HCl and H2O2The oxygen being mixed with the volume ratio of 10:1:1
Change solution and impregnate 5min reaction, aoxidizes polydimethylsiloxanefilm film surface, then rinse 10min with deionized water, then use second
Alcohol rinses 5min, nitrogen drying；(2) polydimethylsiloxanefilm film is put into second alcohol and water to add in the mixed solution of 25:1
30min is reacted after entering 10%APTES, is dried through nitrogen；(3) 15mM Tris buffer solution is prepared using distilled water, and by adding
Enter HCl and pH is maintained 8.5, polydimethylsiloxanefilm film is put into containing 5mg mL-1It is stirred in the solution of dopamine hydrochloride
It after mixing for 24 hours, is dried wash with distilled water through nitrogen, obtains hydrophily polydimethylsiloxanefilm film.
Step 3, the preparation of luminescent layer solution, specific method step include:
(1) 1g dimethyl silicone polymer solution is weighed, 0.1g curing agent, 2g luminescent powder, 0.5g barium titanate is added, utilizes magnetic
Said mixture is sufficiently stirred in power blender, places it in static 20min in vacuum drying oven.
Step 4, the preparation of nano-cellulose suspension, specific method step include:
(1) NaOH for weighing 101.78g is added in the stirring distilled water of 200mL, after NaOH is completely dissolved, Xiang Fanying
The bleached wood pulp cellulose powder that 20g is crushed is added in system, filters after reacting 4h to the close neutrality of pH；(2) configure 200g's
65% H2SO4Solution；(3) oil bath is warming up to 44-45 DEG C, by configured H2SO4Solution is put into oil bath, to H2SO4
Solution is consistent with oil bath temperature.To H2SO4It is slowly added to the wood pulp cellulose powder handled by NaOH in solution, utilizes stirring
Paddle adds water to terminate reaction after stirring 1h always；(4) cellulose that is acid hydrolysis for terminating reaction is poured into beaker, it is quiet that distilled water is added
It after only settling several times, is poured into bag filter, dialysis to neutrality is taken out；(5) ultrasonic under 300W power in ice-water bath
30-60min removes acidolysis cellulose to be cellulose nano-fibrous, and the cellulose nano-fibrous suspension being prepared is placed on
Stored under refrigeration is spare in refrigerator, that is, prepares nano-cellulose suspension.
Step 5, the preparation of nano-cellulose-silver nanowires suspension is mixed, specific method step includes:
(1) by 10mg mL-1Silver nanowires solution adds distilled water to be diluted to 1.5mg mL-1Silver nanowires solution；(2) one is taken
1.5mg mL is added in the 35wt% that quantitative nano-cellulose suspension accounts for silver nanowires solid content-1Silver nanowires solution, in room
The lower magnetic agitation 1h of temperature, to form uniform and stable electrically conductive composite suspension.
Step 6, nano-cellulose-silver nanowires combination electrode prepares the preparation of stretchable electroluminescent device, specific
Method and step includes:
(1) the electrically conductive composite suspension spray of 2.5ml is drawn in hydrophilic poly- two be placed on 60 DEG C of warm tables
On methylsiloxane film, bottom composite conductive layers are obtained, similarly, preparation top composite conductive layers；(2) luminescent layer solution is revolved
It is coated on the composite conductive layers of bottom, is placed on 5min in 80 DEG C of baking ovens；(3) on the light-emitting layer by the lamination of top composite conductive layers,
Copper strips is accessed in bottom, top composite conductive layers to get stretchable electroluminescent device is arrived.
Fig. 1 is the resulting nano-cellulose of embodiment 2-silver nanowires composite conductive film scanning electron microscope (SEM) photograph, shows nanometer
Cellulose-silver nanowires composite conductive film forms uniform and stable, not oxidized conductive network structure.Fig. 2 embodiment 2 is resulting
Nano-cellulose-silver nanowires composite conductive film atomic force microscopy diagram, shows that the addition of nano-cellulose significantly reduces
Nano-cellulose-silver nanowires composite conductive film roughness.Fig. 3 is nano-cellulose-obtained by different nanofiber cellulose contents
The light transmittance and sheet resistance figure of silver nanowires composite conductive film, show light transmittance of the addition for composite conductive film of nano-cellulose
Very little is influenced with sheet resistance.Fig. 4 is the resulting nano-cellulose of embodiment 2-silver nanowires composite conductive film and nanofiber is not added
The time of the silver nanowires conductive film of element and the curve graph of sheet resistance, show the addition of nano-cellulose, so that silver nanowires is led
It is electrically highly stable, without causing sheet resistance linearly increasing because being exposed to room temperature for a long time.Fig. 5 is the resulting nanometer of embodiment 2
Cellulose-silver nanowires mixed liquor is sprayed on the silver nanoparticle that nano-cellulose in hydrophily dimethyl silicone polymer substrate and is not added
Adhesiveness curve graph of the line solution spraying in hydrophily dimethyl silicone polymer substrate, shows the addition of nano-cellulose, mentions
High adhesiveness of the conductive film to substrate.Fig. 6 is the stretchable electroluminescent cell of the resulting composite conducting film layer of embodiment 2 preparation
Brightness variation curve figure and pictorial diagram of the part under different conditions, show nano-cellulose-silver nanowires composite conducting film layer system
Brightness of the standby stretchable electroluminescent device under different conditions is unchanged.
The technical means disclosed in the embodiments of the present invention is not limited only to technological means disclosed in above embodiment, further includes
Technical solution consisting of any combination of the above technical features.It should be pointed out that for those skilled in the art
For, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also considered as
Protection scope of the present invention.
Claims (8)
1. a kind of based on nano-cellulose-silver nanowires electroluminescent device, which is characterized in that be prepared by following steps
It arrives:
A, using dimethyl silicone polymer as raw material, polydimethylsiloxanefilm film is prepared；
B, using polydimethylsiloxanefilm film as raw material, hydrophily polydimethylsiloxanefilm film is prepared；
C, using dimethyl silicone polymer, luminescent powder, barium titanate as raw material, luminescent layer solution is prepared；
D, using bleached wood pulp fiber as raw material, nano-cellulose suspension is prepared；
E., the mixed liquor of nano-cellulose suspension Yu aqueous silver nanowires dispersion liquid is prepared；
F., the obtained mixed liquor of step e is sprayed on hydrophily polydimethylsiloxanefilm film surface, spin coating made from step b
Luminescent layer solution made from step c, in one layer of electrode of top laminate to get based on the electroluminescent hair of nano-cellulose-silver nanowires
Optical device.
2. as described in claim 1 based on nano-cellulose-silver nanowires electroluminescent device, which is characterized in that step a
The preparation method of middle polydimethylsiloxanefilm film adds the following steps are included: (1) weighs 1~10g dimethyl silicone polymer solution
Said mixture is sufficiently stirred using magnetic stirring apparatus in the curing agent for entering 0.1~1g, weighs 1~10g mixing drop-coated in glass
On piece levelling solidifies 30~120min in 40~80 DEG C of baking oven, removes from sheet glass；It is prepared with same method another
Piece polydimethylsiloxanefilm film.
3. as described in claim 1 based on nano-cellulose-silver nanowires electroluminescent device, which is characterized in that step b
The preparation method of middle hydrophily polydimethylsiloxanefilm film the following steps are included:
(1) polydimethylsiloxanefilm film is placed in 5~30min in the oxidation solution immersion of hydrochloric acid and hydrogen peroxide composition, oxygen
Change solution H2O, HCl and H2O2It is mixed with the volume ratio of 2:1:1~10:1:1, aoxidizes polydimethylsiloxanefilm film table
Then face rinses 1~10min with deionized water, then rinses 1~10min, nitrogen drying with ethyl alcohol；
(2) by polydimethylsiloxanefilm film be put into the mixed solution with second alcohol and water be added APTES after reaction 30~
60min, the volume ratio of second alcohol and water is 10:1~25:1 in mixed solution, and APTES accounts for the hundred of the gross mass of ethyl alcohol and aqueous solution
Divide than being 2~10%, is dried through nitrogen；
(3) 8~15mM Tris buffer solution is prepared using distilled water, and pH is maintained 8~8.5 by the way that HCl is added, will gathered
Dimethyl siloxane film is put into containing 1~5mg mL-1In the solution of dopamine hydrochloride stirring 12~for 24 hours after, with distillation
Water cleaning is dried through nitrogen, obtains hydrophily polydimethylsiloxanefilm film.
4. as described in claim 1 based on nano-cellulose-silver nanowires electroluminescent device, which is characterized in that step c
The preparation method of middle luminescent layer solution the following steps are included:
(1) 1~10g dimethyl silicone polymer solution is weighed, 0.1~1g curing agent, 2~20g luminescent powder, 0.5~5g titanium is added
Said mixture is sufficiently stirred using magnetic stirring apparatus in sour barium, places it in static 20~60min in vacuum drying oven.
5. as described in claim 1 based on nano-cellulose-silver nanowires electroluminescent device, which is characterized in that step d
The preparation method of middle nano-cellulose suspension the following steps are included:
(1) NaOH for weighing 25.45~101.78g is added in the stirring distilled water of 100~400mL, is completely dissolved to NaOH
Afterwards, the bleached wood pulp cellulose powder that 5~20g is crushed is added into reaction system, react filter after 2~8h to pH 8~
8.5；
(2) H of 60~65wt% of 50~200g is configured2SO4Solution；
(3) oil bath is warming up to 44-45 DEG C, by configured H2SO4Solution is put into oil bath, to H2SO4Solution and oil bath temperature
Degree is consistent, to H2SO4It is slowly added to the wood pulp cellulose powder handled by NaOH in solution, stirs 30 always using agitating paddle
After~120min plus water terminates reaction；
(4) cellulose that is acid hydrolysis for terminating reaction is poured into beaker, after distilled water quiescent settling is added several times, is poured into
It analyses in bag, dialysis to neutrality is taken out；
(5) in ice-water bath, ultrasound 30-60min removes acidolysis cellulose for cellulose Nanowire under 200~400W power
It is spare to be placed on stored under refrigeration in refrigerator, that is, it is outstanding to prepare nano-cellulose by dimension for the fiber nanofiber suspension being prepared
Supernatant liquid.
6. as described in claim 1 based on nano-cellulose-silver nanowires electroluminescent device, which is characterized in that step e
The preparation method of the mixed liquor of middle nano-cellulose suspension and silver nanowires solution the following steps are included:
(1) by 1~10mg mL-1Silver nanowires solution adds distilled water to be diluted to 0.2~1.5mg mL-1Silver nanowires solution；
(2) it weighs nano-cellulose suspension and 0.2~1.5mg mL is added-1Silver nanowires solution, the additional amount of nano-cellulose
For 5~35wt% of silver nanowires solid content, 30~120min of magnetic agitation, multiple to form uniform and stable conduction at room temperature
Close object suspension.
7. as described in claim 1 based on nano-cellulose-silver nanowires electroluminescent device, which is characterized in that step f
Middle nano-cellulose-silver nanowires combination electrode prepare the preparation method of stretchable electroluminescent device the following steps are included:
(1) draw 0.5~2.5ml electrically conductive composite suspension spray be placed on it is hydrophilic on 40~60 DEG C of warm tables
In polydimethylsiloxanefilm film, bottom composite conductive layers are obtained, similarly, preparation top composite conductive layers；
(2) luminescent layer solution is spin-coated on the composite conductive layers of bottom, is placed on 5~10min in 40~80 DEG C of baking ovens；
(3) on the light-emitting layer by the lamination of top composite conductive layers, in bottom, top composite conductive layers access copper strips to get to can
Stretch electroluminescent device.
8. a kind of application based on nano-cellulose-silver nanowires electroluminescent device, which is characterized in that by claim 1-
Based on nano-cellulose-silver nanowires electroluminescent device applications in flexible display screen or the electricity that shines described in 7 any one
In sub- skin.
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