CN109897377A - A kind of flexible parent metal and preparation method thereof - Google Patents
A kind of flexible parent metal and preparation method thereof Download PDFInfo
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- CN109897377A CN109897377A CN201910211881.4A CN201910211881A CN109897377A CN 109897377 A CN109897377 A CN 109897377A CN 201910211881 A CN201910211881 A CN 201910211881A CN 109897377 A CN109897377 A CN 109897377A
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Abstract
The embodiment of the present invention provides a kind of flexible parent metal and preparation method thereof, is related to flexible electronic device production field, is able to solve existing flexible parent metal complex manufacturing technology, the problem that cost of manufacture is higher and product yield is lower.The production method includes: to be coated with polyamic acid solution on a support, and use the first baking process baking polyamic acid solution to form Polyamic Acid Film；It is coated with oxide sol on Polyamic Acid Film, and uses the second baking process baking oxide sol to form oxide gel film；Polyamic Acid Film and oxide gel film are toasted using third baking process, to form polyimide/oxide film layer, and the multiple groups polyimide/oxide film layer that one group or lamination are arranged is as flexible parent metal.The present invention is for making flexible parent metal.
Description
Technical field
The present invention relates to flexible electronic device production fields more particularly to a kind of flexible parent metal and preparation method thereof.
Background technique
In recent years due to the continuous development of science and technology, requirement of the people to display device not only rests on image quality, response
In terms of the characteristics such as speed, and the requirement to (foldable as soft, rollable etc.) in terms of the form of display device is also increasingly
It is high.Currently, the production of flexible display (such as AMOLED) is usually that first the precursor solution of polymer is coated on hard carrier,
Then flexible parent metal is converted to by heat treatment mode appropriate (such as low-temperature bake and high-temperature baking), then on flexible parent metal
Make driving element and display element, then be packaged technique, finally total is peeled from hard carrier to be formed it is soft
Property display.
However, the oxygen characteristic that blocks water of the existing flexible parent metal by polymeric material is poor, water vapor transmittance
(WVTR) with OTR oxygen transmission rate (O2TR) general all 100~102Magnitude, and OLED device is to WVTR and O2The requirement of TR is distinguished
It is 10-6g·m-2d-1With 10-5cm3·m-2d-1.Therefore, in the prior art it is generally necessary to make single layer on the surface of flexible parent metal
Or the inorganic water oxygen barrier layer of multilayer, such as silicon oxide layer, silicon nitride layer etc..The production of inorganic water oxygen barrier layer generally uses PECVD
(Plasma Enhanced Chemical Vapor Deposition, plasma enhanced chemical vapor deposition method) or ALD
The method of (Atomic layer deposition, atomic layer deposition) needs expensive vacuum equipment, causes to be fabricated in this way
This is higher.In addition, the difference due to inorganic material and organic material in structure, mainly leads between inorganic material and organic material
Physical action combination is crossed, with the increase of inorganic film quantity or thickness, film layer residual stress increases, while polymer material
The problems such as thermal expansion coefficient is higher, these are all easy to cause flexible base board warpage, and inorganic layer removing is failed, it is good in turn result in product
Rate is lower.
Summary of the invention
The embodiment of the present invention provides a kind of flexible parent metal and preparation method thereof, is able to solve existing flexible parent metal production work
The problem that skill is complicated, cost of manufacture is higher and product yield is lower.
In order to achieve the above objectives, the embodiment of the present invention adopts the following technical scheme that
On the one hand, the embodiment of the present invention provides a kind of production method of flexible parent metal, and the production method includes: to support
Polyamic acid solution is coated on object, and it is thin to form polyamic acid to use the first baking process to toast the polyamic acid solution
Film；Oxide sol is coated on the Polyamic Acid Film, and use the second baking process toast the oxide sol with
Form oxide gel film；The Polyamic Acid Film and the oxide gel film are toasted using third baking process,
To form polyimide/oxide film layer, and polyimide/oxide film layer described in the multiple groups that one group or lamination are arranged as
The flexible parent metal.
Optionally, it is described use the second baking process to toast the oxide sol with formed oxide gel film it
Afterwards, the production method further include: be coated with polyamic acid solution on the oxide gel film, and dried using described first
Curing process toasts the polyamic acid solution to form Polyamic Acid Film；It is described that the polyamides is toasted using third baking process
Amino acid film and the oxide gel film to form polyimide/oxide film layer, and one group or lamination are arranged more
The group polyimide/oxide film layer is specifically included as the flexible parent metal: described poly- using the baking of third baking process
Amic acid film and the oxide gel film, to form polyimide/oxide/polyimide film, and by one group or
Polyimide/oxide/polyimide film described in the multiple groups of lamination setting is as the flexible parent metal.
It is optionally, described that the Polyamic Acid Film and the oxide gel film are toasted using third baking process,
To form polyimide/oxide film layer, and polyimide/oxide film layer described in the multiple groups that one group or lamination are arranged as
The flexible parent metal specifically includes: toasting the Polyamic Acid Film using third baking process and the oxide gel is thin
Film, to form polyimide/oxide film layer；It is coated with polyamic acid solution in the polyimide/oxide film layer, and is adopted
The polyamic acid solution is toasted with first baking process to form Polyamic Acid Film；It is toasted using third baking process
The Polyamic Acid Film, to form polyimide/oxide/polyimide film, and the multiple groups that one group or lamination are arranged
Polyimide/oxide/the polyimide film is as the flexible parent metal.
Optionally, first baking process include: in 200 DEG C of nitrogen or inert gas environment below volatilization described in
50% or more solvent in polyamic acid solution.
Optionally, second baking process include: in 200 DEG C of nitrogen or inert gas environment below with 1 DEG C/
Min~5 DEG C/min heating rate is heated up stage by stage come the solvent in the oxide sol that volatilizees.
Optionally, the third baking process includes: in nitrogen or inert gas environment with 3 DEG C/min~10 DEG C/min
Heating rate be warming up to preset temperature stage by stage, and on the preset temperature continue preset duration；Wherein, the default temperature
Degree is greater than or equal to 300 DEG C.
Optionally, the oxide is SiO2、Al2O3、MgO2、ZnO、ZrO2In any one or any several mixing
Object.
Optionally, above support is glass substrate or flexible stainless steel coiled material.
On the other hand, the embodiment of the present invention provides a kind of flexible parent metal, and the flexible parent metal is as described in any one of the above
The production method of flexible parent metal be made.
Flexible parent metal provided in an embodiment of the present invention and preparation method thereof, the production method include: to apply on a support
Cloth polyamic acid solution, and use the first baking process baking polyamic acid solution to form Polyamic Acid Film；In polyamide
It is coated with oxide sol on sour film, and uses the second baking process baking oxide sol to form oxide gel film；
Polyamic Acid Film and oxide gel film are toasted using third baking process, to form polyimide/oxide film layer, and
The multiple groups polyimide/oxide film layer that one group or lamination are arranged is as flexible parent metal.Compared to the prior art, the present invention is real
It applies in example by using third baking process while toasting Polyamic Acid Film and oxide gel film, to form polyamides Asia
Amine/oxide membranous layer, since polyamic acid imidization and oxide precursor object hydrolysis-condensation carry out simultaneously, storeroom mutually expands
It dissipates, the nature transition of film layer interface, so that residual stress is small between film layer, adhesion is good, and oxide diffusion can effectively drop
The thermal expansion coefficient of oligomeric polyimide improves its glass transition temperature, and has efficient water vapor barrier property, improves in this way
The water oxygen barrier properties of flexible parent metal.In addition, due to not needing vacuum equipment in the embodiment of the present invention, so that flexible parent metal
Manufacture craft it is relatively simple, cost of manufacture is lower.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is the production method flow chart of flexible parent metal provided in an embodiment of the present invention；
Fig. 2 be another embodiment of the present invention provides flexible parent metal production method flow chart；
Fig. 3 is the production method flow chart for the flexible parent metal that yet another embodiment of the invention provides；
Fig. 4 is the structural schematic diagram that flexible parent metal is formed on supporter provided in an embodiment of the present invention；
Fig. 5 is the structural schematic diagram provided in an embodiment of the present invention that flexible parent metal is made of roll-to-roll mode.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
The embodiment of the present invention provides a kind of production method of flexible parent metal, as shown in Figure 1 and Figure 5, the production method packet
It includes:
Step 101 is coated with polyamic acid solution on a support, and toasts polyamic acid solution using the first baking process
To form Polyamic Acid Film.
Above support can be the glass substrate of hard, be also possible to flexible stainless steel coiled material, the embodiment of the present invention
Material, form for supporter etc. are without limitation.
The embodiment of the present invention for coating mode also without limitation, it is exemplary, can be slit (slit/slot die)
Coating method, scraper (blade) coating method, spraying (spray) etc..
Polyamic acid (PAA) film can be formed using the first baking process baking polyamic acid (PAA) solution；Described
One baking process is low-temperature bake, specifically, the polyamides that can volatilize in 200 DEG C of nitrogen or inert gas environment below
50% or more solvent in amino acid solution, to form PAA film.
Step 102 is coated with oxide sol on Polyamic Acid Film, and molten using the second baking process baking oxide
Glue is to form oxide gel film.
Oxide in the oxide sol can be SiO2、Al2O3、MgO2、ZnO、ZrO2In any one or appoint
It anticipates several mixtures, it is not limited in the embodiment of the present invention.
Oxide gel film can be formed using the second baking process baking oxide sol；Second baking process
For low-temperature bake, specifically, can be in 200 DEG C of nitrogen or inert gas environment below with 1 DEG C/min~5 DEG C/min liter
Warm rate is heated up stage by stage come the solvent in the oxide sol that volatilizees, to form oxide gel film.
Step 103 toasts Polyamic Acid Film and oxide gel film using third baking process, to form polyamides Asia
Amine/oxide membranous layer, and the multiple groups polyimide/oxide film layer that one group or lamination are arranged is as flexible parent metal.
Polyamic acid (PAA) film and oxide gel film are toasted using third baking process, polyamides Asia can be formed
Amine (PI)/oxide membranous layer；The third baking process is high-temperature baking, specifically, can be in nitrogen or inert gas environment
In preset temperature is warming up to stage by stage with 3 DEG C/min~10 DEG C/min heating rate, and continue on the preset temperature pre-
If duration；Wherein, the preset temperature is greater than or equal to 300 DEG C；The preset duration is pre-set duration, this field skill
Setting when art personnel can carry out according to the actual situation, it is not limited in the embodiment of the present invention.
It is exemplary, PAA solution can be coated on a support first, in 40 DEG C~120 DEG C nitrogen or inert gas environment
The middle solvent by PAA solution evaporates into 50% or more to form PAA film；Then it is thin oxide sol to be coated on the PAA
On film, using sol-gel technology with 1 DEG C/min~5 DEG C/min heating rate sublevel in nitrogen or inert gas environment
Duan Shengwen is come the solvent in the oxide sol that volatilizees to form oxide gel film；Again with 3 DEG C/min~10 DEG C/min liter
Warm rate is warming up to 450 DEG C stage by stage and maintains preset duration, so that the imidization of PAA and the generation of sull are complete simultaneously
At.Can as needed above steps may be repeated multiple times to make multilayer film as flexible parent metal.Before PAA imidization and oxide
It drives object hydrolysis-condensation to carry out simultaneously, storeroom phase counterdiffusion, the nature transition of film layer interface, residual stress is small between film layer, adhesion
It is good, and oxide diffusion can effectively reduce the thermal expansion coefficient (CTE) of PI, improve its glass transition temperature (Tg), and have
There is efficient water vapor barrier property.
This method not only can chip (sheet to sheet) production, be more suitable for the height of roll-to-roll (roll to roll)
Imitate production method.
Example goes out a specific embodiment of chip production below: being coated on the glass substrate using the method for slot coated
Then one layer of PAA solution toasts solvent flashing to 65% in 60 DEG C of nitrogen environment, forms PAA film；Then in formation
One layer of SiO of slot coated is used on PAA film2Colloidal sol, heated up in nitrogen environment with the rate of 2 DEG C/min baking shape stage by stage
At SiO2Gel film, it is specific: to continue 30min at 30 DEG C, then heat to 60 DEG C, continue 20min at 60 DEG C, then
90 DEG C are warming up to, continues 15min at 90 DEG C；And then baking is heated up stage by stage with the rate of 5 DEG C/min to form PI/ oxidation
Object film layer, it is specific: after being warming up to 120 DEG C, to continue 15min at 120 DEG C, then heat to 240 DEG C, continue at 240 DEG C
15min then heats to 480 DEG C, continues 30min at 480 DEG C, to complete the imidization of PAA and the generation of sull,
So far PI/SiO is formed2Flexible parent metal.It is subsequent can be in the PI/SiO of formation2Driving element, display device, envelope are made in film layer
Dress etc., finally removes it from glass substrate, forms flexible display device.
Example goes out a specific embodiment of roll-to-roll production below: refering to what is shown in Fig. 5, using step 101 in 50um thickness
Stainless steel coiled material on using slot coated method be coated with one layer of PAA solution, then toast and wave in 60 DEG C of nitrogen environment
The solvent in PAA solution is sent out to 80%, forms PAA film；Then slit is used on the PAA film of formation using step 102
It is coated with one layer of SiO2Colloidal sol, the baking that then heated up stage by stage in nitrogen environment with the rate of 2 DEG C/min form SiO2Gel is thin
Film, specific: continue 30min at 30 DEG C, then heat to 60 DEG C, continues 20min at 60 DEG C, then heat to 90 DEG C,
Continue 15min at 90 DEG C；Finally utilize step 103 by the PAA/SiO of formation2Gel film is taken off from stainless-steel roll material,
And the baking that heated up stage by stage with the rate of 5 DEG C/min is to form PI/SiO2Film layer, it is specific: after being warming up to 120 DEG C, at 120 DEG C
Shi Chixu 15min then heats to 240 DEG C, continues 15min at 240 DEG C, then heats to 480 DEG C, continues at 480 DEG C
30min so far forms PI/SiO to complete the imidization of PAA and the generation of sull2Coiled material.
Another embodiment of the present invention provides a kind of production methods of flexible parent metal, as shown in Fig. 2, the production method packet
It includes:
Step 201 is coated with polyamic acid solution on a support, and toasts polyamic acid solution using the first baking process
To form Polyamic Acid Film.
It is exemplary, refering to what is shown in Fig. 4, being coated with one layer of PAA solution using the method for slot coated on glass substrate 11, so
Solvent flashing is toasted in 60 DEG C of nitrogen environment afterwards to 65%, forms PAA film 12.
Step 202 is coated with oxide sol on Polyamic Acid Film, and molten using the second baking process baking oxide
Glue is to form oxide gel film.
It is exemplary, refering to what is shown in Fig. 4, using one layer of SiO of slot coated on PAA film 122-Al2O3Then colloidal sol exists
It heats up to toast stage by stage with the rate of 2 DEG C/min in nitrogen environment and forms SiO2-Al2O3Gel film 13, it is specific: at 30 DEG C
Shi Chixu 30min then heats to 60 DEG C, continues 20min at 60 DEG C, then heats to 90 DEG C, continues at 90 DEG C
15min。
Step 203 is coated with polyamic acid solution on oxide gel film, and toasts polyamides using the first baking process
Amino acid solution is to form Polyamic Acid Film.
It is exemplary, refering to what is shown in Fig. 4, in SiO2-Al2O3One layer is coated with using the method for slot coated on gel film 13
Then PAA solution toasts solvent flashing to 65% in 60 DEG C of nitrogen environment, forms PAA film 12.
Step 204 toasts Polyamic Acid Film and oxide gel film using third baking process, to form polyamides Asia
Amine/oxide/polyimide film, and multiple groups polyimide/oxide/polyimide film that one group or lamination are arranged is made
For flexible parent metal.
It is exemplary, refering to what is shown in Fig. 4, heated up stage by stage with the rate of 5 DEG C/min baking PAA film 12 and SiO2-Al2O3
Gel film 13, it is specific: after being warming up to 120 DEG C, to continue 15min at 120 DEG C, 240 DEG C are then heated to, at 240 DEG C
Continue 15min, then heat to 480 DEG C, continue 30min at 480 DEG C, to complete imidization and the sull of PAA
It generates, so far forms PI/SiO2-Al2O3/ PI flexible parent metal.
Yet another embodiment of the invention provides a kind of production method of flexible parent metal, as shown in figure 3, the production method packet
It includes:
Step 301 is coated with polyamic acid solution on a support, and toasts polyamic acid solution using the first baking process
To form Polyamic Acid Film.
Step 302 is coated with oxide sol on Polyamic Acid Film, and molten using the second baking process baking oxide
Glue is to form oxide gel film.
Step 303 toasts Polyamic Acid Film and oxide gel film using third baking process, to form polyamides Asia
Amine/oxide membranous layer.
Step 304 is coated with polyamic acid solution in polyimide/oxide film layer, and is dried using the first baking process
Polyamic acid solution is baked to form Polyamic Acid Film.
Step 305 toasts Polyamic Acid Film using third baking process, sub- to form polyimide/oxide/polyamides
Amine film layer, and multiple groups polyimide/oxide/polyimide film that one group or lamination are arranged is as flexible parent metal.
PI/ oxide/PI film layer can be also produced using such production method.
Another embodiment of the present invention provides a kind of flexible parent metal, flexible parent metal flexibility as described in any one of the above
The production method of substrate is made.
The embodiment of the present invention toasts Polyamic Acid Film when making flexible parent metal, by using third baking process simultaneously
With oxide gel film, to form polyimide/oxide film layer, due to polyamic acid imidization and oxide precursor object water
Solution-polycondensation carries out simultaneously, storeroom phase counterdiffusion, the nature transition of film layer interface, so that residual stress is small between film layer, adheres to
Property it is good, and oxide diffusion can effectively reduce the thermal expansion coefficient of polyimides, improve its glass transition temperature, and have
Efficient water vapor barrier property improves the water oxygen barrier properties of flexible parent metal in this way.In addition, due to being not required in the embodiment of the present invention
Want vacuum equipment, so that the manufacture craft of flexible parent metal is relatively simple, and cost of manufacture is lower.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by those familiar with the art, all answers
It is included within the scope of the present invention.Therefore, protection scope of the present invention should be with the scope of protection of the claims
It is quasi-.
Claims (9)
1. a kind of production method of flexible parent metal, which is characterized in that the production method includes:
It is coated with polyamic acid solution on a support, and it is poly- to be formed to use the first baking process to toast the polyamic acid solution
Amic acid film；
Oxide sol is coated on the Polyamic Acid Film, and use the second baking process toast the oxide sol with
Form oxide gel film；
The Polyamic Acid Film and the oxide gel film are toasted using third baking process, with formed polyimides/
Oxide membranous layer, and polyimide/oxide film layer described in the multiple groups that one group or lamination are arranged is as the flexible parent metal.
2. the production method of flexible parent metal according to claim 1, which is characterized in that use the second baking process described
After the oxide sol is toasted to form oxide gel film, the production method further include:
It is coated with polyamic acid solution on the oxide gel film, and the polyamides is toasted using first baking process
Amino acid solution is to form Polyamic Acid Film；
It is described that the Polyamic Acid Film and the oxide gel film are toasted using third baking process, to form polyamides Asia
Amine/oxide membranous layer, and polyimide/oxide film layer described in the multiple groups that one group or lamination are arranged is as the flexible parent metal
It specifically includes:
The Polyamic Acid Film and the oxide gel film are toasted using third baking process, with formed polyimides/
Oxide/polyimide film, and polyimide/oxide/polyimide film described in the multiple groups that one group or lamination are arranged
As the flexible parent metal.
3. the production method of flexible parent metal according to claim 1, which is characterized in that described to be dried using third baking process
The Polyamic Acid Film and the oxide gel film are baked, to form polyimide/oxide film layer, and it is by one group or folded
Polyimide/oxide film layer described in the multiple groups of layer setting is specifically included as the flexible parent metal:
The Polyamic Acid Film and the oxide gel film are toasted using third baking process, with formed polyimides/
Oxide membranous layer；
It is coated with polyamic acid solution in the polyimide/oxide film layer, and institute is toasted using first baking process
Polyamic acid solution is stated to form Polyamic Acid Film；
The Polyamic Acid Film is toasted using third baking process, to form polyimide/oxide/polyimide film,
And polyimide/oxide/polyimide film described in the multiple groups that one group or lamination are arranged is as the flexible parent metal.
4. the production method of flexible parent metal as claimed in any of claims 1 to 3, which is characterized in that described first
Baking process includes:
Volatilize in the polyamic acid solution in 200 DEG C of nitrogen or inert gas environment below 50% or more solvent.
5. the production method of flexible parent metal according to claim 1, which is characterized in that second baking process includes:
It heats up to come stage by stage with 1 DEG C/min~5 DEG C/min heating rate in 200 DEG C of nitrogen or inert gas environment below
The solvent to volatilize in the oxide sol.
6. the production method of flexible parent metal as claimed in any of claims 1 to 3, which is characterized in that the third
Baking process includes:
Preset temperature is warming up to stage by stage with 3 DEG C/min~10 DEG C/min heating rate in nitrogen or inert gas environment,
And continue preset duration on the preset temperature；Wherein, the preset temperature is greater than or equal to 300 DEG C.
7. the production method of flexible parent metal according to claim 1, which is characterized in that the oxide is SiO2、Al2O3、
MgO2、ZnO、ZrO2In any one or any several mixture.
8. the production method of flexible parent metal according to claim 1, which is characterized in that above support be glass substrate or
Flexible stainless steel coiled material.
9. a kind of flexible parent metal, which is characterized in that flexible parent metal flexibility as described in any one of claim 1 to 8
The production method of substrate is made.
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Cited By (1)
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| CN114335404A (en) * | 2021-12-20 | 2022-04-12 | 深圳市华星光电半导体显示技术有限公司 | Preparation method of flexible substrate, flexible substrate and flexible display panel |
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| CN109897377B (en) | 2021-04-30 |
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