CN110257003A - Transferable transparent flexible conductive adhesive film of tack and its preparation method and application - Google Patents
Transferable transparent flexible conductive adhesive film of tack and its preparation method and application Download PDFInfo
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- CN110257003A CN110257003A CN201910529991.5A CN201910529991A CN110257003A CN 110257003 A CN110257003 A CN 110257003A CN 201910529991 A CN201910529991 A CN 201910529991A CN 110257003 A CN110257003 A CN 110257003A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/10—Adhesives in the form of films or foils without carriers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0806—Silver
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2483/00—Presence of polysiloxane
Abstract
The invention belongs to electronic information technical fields, specially transferable transparent flexible conductive adhesive film of tack and its preparation method and application.Preparation method of the present invention includes: the pretreatment of polytetrafluoro substrate, as PDMS glue film substrate, prepares silver nanowires network, transfer transparent flexible conductive adhesive film transfer etc. in PDMS film surface.Prepared adhesive film material inherits the transparent conductivity of silver nanowires network well, thickness can regulate and control between 1 ~ 10 micron, have the advantage that (1) adapts to the shape of electrode contact material, roughness, hydrophilic and hydrophobic height compared with existing transparent conductive material；(2) there is tack, it is small to contact material surface damage, it is easy to secondary transferring separation, while guaranteeing good physical contact and electrical contact；(3) there is low-crackle sensitive, be not easy to form electrode leakage because of contact material micro-crack defect, lead to shorted devices.It thus can be widely applied in the constructing of various flexible electronic devices and micro-nano device.
Description
Technical field
The invention belongs to electronic information technical fields, and in particular to the transferable transparent flexible conductive adhesive film of tack and its system
Standby and application.
Background technique
The preparation of transparent flexible conductive material and its application in terms of electronic device are that flexible electronic field is ground in recent years
The hot spot studied carefully is the critical material for developing flexible display, photovoltaic and photoelectric detection equipment.The oxidation being most widely used at present
The ceramic bases transparent conductive material brittleness such as indium tin (ITO) is larger, is easy to stress embrittlement, is unable to satisfy the need of flexible electronic devices
It asks.The needs of transparent flexible conduction may be met well with the metal nanometer line network that silver nanowires (Ag NW) is representative, but
Its transparency tends to rely on uniform solution spin-coating process, and the hydrophily and anti-solvent aggressivity to contact material have higher
Requirement, limit when constructing device material selection.Although and can be real currently based on the pre- spin-coating film of hydrophily PET substrate
Existing higher transparent conductivity, is but difficult to form good physical contact between electronic material.The present invention proposes that one kind is based on
The transferable transparent flexible conductive adhesive film of the tack of metal nanometer line, prepares PDMS- polytetrafluoro substrate first, carry out later etc. from
Daughter hydrophilic treated, and spin coating metal nanometer line obtain the electrically conducting transparent flexibility glue film for being easy to shift.Compared to conventional method,
The electrically conducting transparent flexibility glue film of this method preparation while keeping compared with high transparency electric conductivity, also have it is good from tackness,
Can directly be formed with a variety of materials it is good physically and electrically contact, while to material surface destroy it is small, be easy to shift, and have
Lower crack sensitivity can preferably meet the materials demand of flexible wearable electronic equipment.
Summary of the invention
The purpose of the present invention is to provide a kind of transferable transparent flexible conductive adhesive film of the extensive tack of adaptability and its
Preparation method and application.
The transferable transparent flexible conductive adhesive film preparation method of tack provided by the invention, the pre- place including polytetrafluoro substrate
Reason prepares silver nanowires network, transfer transparent flexible conductive adhesive film transfer in PDMS film surface as PDMS glue film substrate
Deng.Specific steps are as follows:
(1) pretreatment of polytetrafluoro substrate: under plane template compacting, 270 ~ 350 DEG C is heated to and keeps the temperature 2 ~ 5 hours, later certainly
It so is cooled to room temperature, planarizing process is carried out to the polytetrafluoro substrate after cleaning；
(2) PDMS host agent, crosslinking agent and toluene are sufficiently mixed according to a certain percentage, obtain solution A；
(3) ethylene glycol, silver nitrate, low molecular weight PVP, high molecular weight PVP and iron chloride are sufficiently mixed according to a certain percentage molten
Solution, obtains solution B；
(4) solution B is heated 2 ~ 4 hours at 130 ~ 150 DEG C, obtains the silk color solution C comprising silver nanowires；
(5) a certain amount of dehydrated alcohol is added to be sufficiently mixed into solution C, 4500 ~ 5500 turns are centrifuged and remove supernatant liquid；
(6) step (5) are repeated repeatedly (generally 3-5 times), to remove the ethylene glycol in solution C, PVP and by-product；
(7) solution A is spin-coated on polytetrafluoro substrate, and keeps the temperature 3 ~ 5 hours at 80 ~ 120 DEG C, form pellosil-polytetrafluoro
Substrate；
(8) pellosil-polytetrafluoro substrate 10 ~ 20 seconds is handled in oxygen plasma atmosphere, carries out surface hydrophilic processing；
(9) solution that step (6) obtains is spin-coated on hydrophilic treated pellosil-polytetrafluoro substrate surface, is formed after dry
The transferable transparent flexible conductive adhesive film of tack.
Further, in solution A, crosslinking agent be DOW CORNING 184,184 mass ratio 10:(0.8 of PDMS host agent and DOW CORNING ~
1.2) it is 25 ~ 35% that, toluene, which accounts for the volume fraction of solution A, and can be by changing PDMS host agent, 184 crosslinking agent of DOW CORNING and toluene
Usage ratio, adjust film thickness.
Further, in solution B, 50 ~ 70 mg/ml silver nitrate ethylene glycol solutions, 7 ~ 8 mg/ml PVP ethylene glycol solutions are (low
Molecular weight: high molecular weight=1:(1.5 ~ 2.5)), 500 ~ 700 μm of ol/L iron chloride ethylene glycol solutions are according to 1:(7.2 ~ 7.4):
The volume ratio of (0.8 ~ 0.85) is uniformly mixed.
In the present invention, use the polytetrafluoro substrate of template processing as recyclable shaped substrate.
In the present invention, by changing toluene ratio in solution A, PDMS film thickness is enable to regulate and control between 1 ~ 10 micron.
It in the present invention, is handled by oxygen plasma surface hydrophilic, enables the silver nanowires of solution growth in PDMS glue film
Surface forms uniform conductive network.
Experiment shows that the transferable transparent flexible conductive adhesive film of tack prepared by the present invention has excellent properties, in reality
While existing high transparency, high conductivity and flexibility, there is good adaptability to different material and shape, surface condition etc.,
It is easy to use simultaneously, it is in electrical contact and is physically contacted and is all right.
The present invention has following outstanding feature:
(1) shape of electrode contact material, roughness, hydrophilic and hydrophobic height are adapted to, can be widely applied to various flexible electronics
In equipment especially flexible wearable optoelectronic device or display equipment, it can also be used in the constructing of micro-nano device；
(2) there is tack, it is small to contact material surface damage, it is easy to secondary transferring separation, while guaranteeing that good physics connects
Touching and electrical contact；
(3) there is low-crackle sensitive, be not easy to form electrode leakage because of contact material micro-crack defect, lead to shorted devices.
Present invention substantive distinguishing features outstanding and marked improvement can be emerged from from following instance, but not limited to this.
Detailed description of the invention
Fig. 1 is tack conductive adhesive film preparation process (a) and its SEM picture (b).
Fig. 2 tack conductive adhesive film and Te micro wire contact schematic diagram and its device iv performance.
Fig. 3 is by top electrode device of tack conductive adhesive film and using silver nanowires as the iv Character Comparison of top electrode device.
Specific embodiment
Specific implementation of the invention is described further below in conjunction with example and attached drawing, but implementation and protection of the invention
It is without being limited thereto.
Embodiment 1
Under plane template compacting, it is heated to 345 DEG C and keeps the temperature 2 hours, room temperature is naturally cooled to later, to poly- four after cleaning
Fluorine substrate carries out planarizing process；According to 184 mass ratio 10:1 of PDMS host agent and DOW CORNING, toluene accounts for the volume fraction of solution A
For 30% configuration solution A；According to 6mg/ml silver nitrate ethylene glycol solution, 7.41 mg/ml PVP ethylene glycol solution (MW55000:
MW1300000=1:2), 600 μm of ol/L iron chloride ethylene glycol solution volume ratio 6:44:5 configure solution Bs；By solution B at 140 DEG C
Lower heating 3 hours, obtains the silk color solution C comprising silver nanowires;It is sufficiently mixed into solution C that a certain amount of dehydrated alcohol is added
It closes, 5500 turns are centrifuged and remove supernatant liquid, repeat the solution C after this step 3 time is cleaned later；Solution A is spin-coated on
On polytetrafluoro substrate, and 4 hours are kept the temperature at 120 DEG C, forms pellosil-polytetrafluoro substrate；In oxygen plasma atmosphere
Pellosil-polytetrafluoro substrate 15 seconds, and the solution C after surface spin coating cleaning are managed, it is transferable transparent to form tack after dry
Compliant conductive glue film.
If Fig. 2 is shown, the sample of separation 3mm*3mm size is cut to the transferable transparent flexible conductive adhesive film of above-mentioned tack
Product.The micro wire sample one end Te is fixed on an insulating substrate using carbon slurry electrode, by a drop dehydrated alcohol drop on micro wire,
Transparent conductive film is clamped with tweezers, tears its polytetrafluoro substrate depended on off, is flattened under the effect of ethyl alcohol drop, in 60 DEG C of drying-plates
Upper heating 30s makes ethyl alcohol volatilize, and transparent conductive film is attached on Te micro wire surface and forms good physical contact.
The resistance situation of sample is tested by multimeter, is observed stable rectifying effect, is passed through semiconductor later
Test macro acquires I-V data information, observes stable current-voltage correlation, electric current has 7 orders of magnitude before and after thermal breakdown
Mutation, and there is clearly breakdown voltage, show to form between transparent flexible conductive adhesive film and Te micro wire sample good
Electrical contact, it was demonstrated that it can be with the irregular contact surface good conformity including micro wire.
Embodiment 2
Under plane template compacting, it is heated to 320 DEG C and keeps the temperature 3 hours, room temperature is naturally cooled to later, to poly- four after cleaning
Fluorine substrate carries out planarizing process；According to 184 mass ratio 10:1 of PDMS host agent and DOW CORNING, toluene accounts for the volume fraction of solution A
For 35% configuration solution A；According to 6mg/ml silver nitrate ethylene glycol solution, 8 mg/ml PVP ethylene glycol solution (MW55000:
MW1300000=1:2), 500 μm of ol/L iron chloride ethylene glycol solution volume ratio 1:7.4:0.85 configure solution Bs；Solution B is existed
It is heated 2.5 hours at 140 DEG C, obtains the silk color solution C comprising silver nanowires;A certain amount of dehydrated alcohol is added into solution C
It is sufficiently mixed, 5000 turns are centrifuged and remove supernatant liquid, repeat the solution C after this step 3 time is cleaned later；By solution A
It is spin-coated on polytetrafluoro substrate, and keeps the temperature 3 hours at 120 DEG C, form pellosil-polytetrafluoro substrate；In oxygen plasma atmosphere
Middle processing pellosil-polytetrafluoro substrate 15 seconds, and the solution C after surface spin coating cleaning are enclosed, forming tack after dry can turn
Move transparent flexible conductive adhesive film.
The sample of separation 5mm*5mm size is cut to the transferable transparent flexible conductive adhesive film of above-mentioned tack.By a piece of N-shaped
Lightly doped silicon wafer is attached in the glass substrate for being coated with indium gallium alloy electrode, by a drop dehydrated alcohol drop in lightly doped silicon wafer table
Transparent conductive film is clamped with tweezers in face, tears its polytetrafluoro substrate depended on off, flattens under the effect of ethyl alcohol drop, at 60 DEG C
30s is heated on drying-plate makes ethyl alcohol volatilize, and transparent conductive film is attached on silicon chip surface and forms good physical contact.
The resistance and commutating ratio of sample are measured and recorded by multimeter, take the electrically conducting transparent glue on surface off with tweezers later
The transparent conductive film torn is attached on ethyl alcohol drop flattens again, 60 by film by a drop dehydrated alcohol drop in silicon chip surface
Heating and formation reason contacts again on DEG C drying-plate, test sample resistance and commutating ratio, not bright with test data before again
Significant difference is other, illustrates that transparent conductive film electrode is easy to secondary transferring separation, and its electrical property and contact situation do not have significant change.
Embodiment 3
Under plane template compacting, it is heated to 300 DEG C and keeps the temperature 4 hours, room temperature is naturally cooled to later, to poly- four after cleaning
Fluorine substrate carries out planarizing process；According to 184 mass ratio 10:1 of PDMS host agent and DOW CORNING, toluene accounts for the volume fraction of solution A
For 25% configuration solution A；According to 6mg/ml silver nitrate ethylene glycol solution, 7.41 mg/ml PVP ethylene glycol solution (MW55000:
MW1300000=1:2), 700 μm of ol/L iron chloride ethylene glycol solution volume ratio 1:7.3:0.80 configure solution Bs；Solution B is existed
It is heated 5 hours at 140 DEG C, obtains the silk color solution C comprising silver nanowires;A certain amount of dehydrated alcohol is added to fill into solution C
Divide mixing, 5500 turns are centrifuged and remove supernatant liquid, repeat the solution C after this step 3 time is cleaned later；Solution A is revolved
It is coated on polytetrafluoro substrate, and keeps the temperature 4 hours at 120 DEG C, form pellosil-polytetrafluoro substrate；In oxygen plasma atmosphere
It is transferable to form tack after dry for middle processing pellosil-polytetrafluoro substrate 20 seconds, and the solution C after surface spin coating cleaning
Transparent flexible conductive adhesive film.
If Fig. 3 is shown, the sample of separation 3mm*3mm size is cut to the transferable transparent flexible conductive adhesive film of above-mentioned tack
Product.Zinc oxide sodium rice film is prepared on conductive substrates surface, take the direct drop coating silver nanowires ethanol solution of a piece of sample and is dried,
Another sample is top electrode using the transparent conductive film of preparation, and concrete operations are similar to previous examples.
Test the I-V data information of two samples respectively using semiconductor test system, direct drop coating silver nanowires solution
Sample short circuit loses photoelectric properties, and uses the sample that transparent conductive film is top electrode working properly, illustrates the transparent of preparation
Conductive adhesive film has low-crackle sensitive, is not easy to form electrode leakage because of contact material micro-crack defect, leads to shorted devices, energy
The electrode for being enough in the porous materials such as micro-nano structure film is constructed.
Claims (7)
1. a kind of preparation method of the transferable transparent flexible conductive adhesive film of tack, which is characterized in that including polytetrafluoro substrate
Pretreatment prepares silver nanowires network in PDMS film surface, transfer transparent flexible conductive adhesive film turns as PDMS glue film substrate
It moves；Specific steps are as follows:
(1) pretreatment of polytetrafluoro substrate: under plane template compacting, 270 ~ 350 DEG C are heated to, keeps the temperature 2 ~ 5 hours, later
Room temperature is naturally cooled to, planarizing process is carried out to the polytetrafluoro substrate after cleaning；
(2) PDMS host agent, crosslinking agent and toluene are sufficiently mixed, obtain solution A；
(3) ethylene glycol, silver nitrate, low molecular weight PVP, high molecular weight PVP and iron chloride are sufficiently mixed dissolution, obtain solution B；
(4) solution B is heated 2 ~ 4 hours at 130 ~ 150 DEG C, obtains the silk color solution C comprising silver nanowires；
(5) dehydrated alcohol is added into solution C, is sufficiently mixed, 4500 ~ 5500 turns are centrifuged and remove supernatant liquid；
(6) step (5) are repeated repeatedly, to remove the ethylene glycol in solution C, PVP and by-product；
(7) solution A is spin-coated on polytetrafluoro substrate, and keeps the temperature 3 ~ 5 hours at 80 ~ 120 DEG C, form pellosil-polytetrafluoro
Substrate；
(8) pellosil-polytetrafluoro substrate 10 ~ 20 seconds is handled in oxygen plasma atmosphere, carries out surface hydrophilic processing；
(9) solution that step (6) obtains is spin-coated on hydrophilic treated pellosil-polytetrafluoro substrate surface, is formed after dry
The transferable transparent flexible conductive adhesive film of tack.
2. preparation method according to claim 1, which is characterized in that in solution A, crosslinking agent is DOW CORNING 184, PDMS master
Mass ratio 10:(0.8 ~ 1.2 of agent and DOW CORNING 184), the volume fraction that toluene accounts for solution A is 25 ~ 35%, and passes through change
The usage ratio of PDMS host agent, crosslinking agent and toluene adjusts film thickness.
3. preparation method according to claim 1 or 2, which is characterized in that solution B is by 50 ~ 70 mg/ml silver nitrate second two
Alcoholic solution, 7 ~ 8mg/ml PVP ethylene glycol solution, 500 ~ 700 μm of ol/L iron chloride ethylene glycol solutions are according to 1:(7.2 ~ 7.4):
The volume ratio of (0.8 ~ 0.85) is uniformly mixed and obtains；Wherein, in PVP ethylene glycol solution, low molecular weight: high molecular weight=1:(1.5
~ 2.5).
4. preparation method according to claim 1, which is characterized in that use 184 crosslinking agent of DOW CORNING, and dropped using toluene
Low solution A viscosity.
5. preparation method according to claim 1, which is characterized in that by changing toluene ratio in solution A, regulate and control PDMS
Film thickness is in 1 ~ 10 micron range.
6. the transferable transparent flexible conductive adhesive film of the tack that the preparation method as described in one of claim 1-5 obtains.
7. the transferable transparent flexible conductive adhesive film of the tack of claim 6 is in flexible electronic devices or during micro-nano device constructs
Application.
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Application publication date: 20190920 |