CN110450326A - A kind of preparation method of flexible screen bright enhancement film substrate - Google Patents
A kind of preparation method of flexible screen bright enhancement film substrate Download PDFInfo
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- CN110450326A CN110450326A CN201910749453.7A CN201910749453A CN110450326A CN 110450326 A CN110450326 A CN 110450326A CN 201910749453 A CN201910749453 A CN 201910749453A CN 110450326 A CN110450326 A CN 110450326A
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- film substrate
- flexible screen
- enhancement film
- bright enhancement
- stalk
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C41/00—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
- B29C41/003—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor characterised by the choice of material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C41/00—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
- B29C41/02—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor for making articles of definite length, i.e. discrete articles
- B29C41/12—Spreading-out the material on a substrate, e.g. on the surface of a liquid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C41/00—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
- B29C41/34—Component parts, details or accessories; Auxiliary operations
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2001/00—Use of cellulose, modified cellulose or cellulose derivatives, e.g. viscose, as moulding material
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- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
The invention proposes a kind of preparation methods of flexible screen bright enhancement film substrate, comprising: S1. crushes dry stalk with micronizer, obtains straw powder, it is dry, aminotriacetic acid, n,N-Dimethylaniline, potassium peroxydisulfate, hydrogen peroxide, normal-temperature continuous stirring is added, filtering, heavy metal chelant, stirring is added in washing, filtering, it is dry；It crushes, sieving obtains pretreated stalk；The pretreated stalk yield is greater than 87%；S2. acetum, ultrasound is added in pretreated stalk, centrifugation takes supernatant, dilution, is evaporated, obtains basement membrane, membrane surface is immersed in acetaldehyde and silane coupler solution, it takes out, surface uniformly coats silver ammino solution, and it is dry, obtain flexible screen bright enhancement film substrate.Preparation method of the present invention is simple, raw material sources are wide, at low cost, and nonconducting stalk is made into the very excellent flexible screen bright enhancement film substrate of mechanical property and electric property, is had a vast market foreground.
Description
Technical field
The present invention relates to flexible material preparation technical fields, and in particular to a kind of preparation side of flexible screen bright enhancement film substrate
Method.
Background technique
Flexible electronic can be summarized as being that organic/inorganic materials electronic device is produced on to flexibility/Drawability plastics or Bao Jin
Belong to the new electronic technology on substrate, with its unique flexibility/ductility and efficient, low cost manufacturing technique, in information, energy
The fields such as source, medical treatment, national defence have wide application prospect, such as flexible electronic displays, Organic Light Emitting Diode OLED, printing
RFID, thin-film solar cell panel, electronics surface mount (Skin Patches) etc..As traditional IC technology, work is manufactured
Skill and equipment are also the main drive of flexible electronic technology development.Flexible electronic manufacturing technology level index includes chip features
Size and substrate area size, key are how on the substrate of more large format to produce characteristic size more with lower cost
Small flexible electronic device.
Currently, bright enhancement film (BEF) is widely used in illuminating module to be used to converge the light that light source is issued, especially supervise
Visual organ etc. is shown in equipment often using the energy of bright enhancement film (BEF) Lai Zengjia display brightness and saving display battery apparatus.Increase
The principle of light film is to be adjusted the light except directive observer visual angle to observer visual angle by reflecting and reflecting, in this way
Just improve the utilization rate of the issued luminous energy of light source.
For organic flexible screen is compared to traditional liquid crystal display, have many advantages, such as, if energy consumption is lower, volume is lighter
Thin, cruise duration is longer, and the service life is longer.Organic flexible screen technology is as a new technology, it is contemplated that 3 to 5 years following
It is interior, it is expected to apply on a large scale on the high-tech products such as mobile phone, LCD TV, computer, automobile and wearable smart machine.Increase
Light film is the significant components of organic flexible screen, and it is mostly chemical industry high molecular polymer etc. that the tradition of bright enhancement film substrate, which prepares raw material, former
Expect that price is high, development is unsustainable.
Summary of the invention
The present invention provides a kind of preparation method of flexible screen bright enhancement film substrate, it is intended that providing a kind of flexible screen increasing
Light film substrate, by the way that using stalk as raw material, the Performances of Novel Nano-Porous meter level obtained after the processing of specific physico-chemical method Jing Guo chemical modification is fine
Chlorins compound is tieed up, the heavy metal ion adsorbed removal contained by heavy metal chelant obtains the higher fiber of purity
Flexible screen bright enhancement film substrate is being prepared, on conductive and mechanical properties in chlorins compound after coating film formation process
There is great raising.
The present invention provides a kind of preparation method of flexible screen bright enhancement film substrate, comprising the following steps:
S1. the pretreatment of stalk: dry stalk is crushed with micronizer, obtains straw powder, dry to constant weight, is added
Enter aminotriacetic acid, n,N-Dimethylaniline, potassium peroxydisulfate, hydrogen peroxide, normal-temperature continuous stirs 10-12h, product filtering, filter
Slag is washed with water to neutrality, soluble in water, and heavy metal chelant is added, is stirred to react 2-5h, filters, filtrate decompression evaporation, vacuum
It is dry；Powder after drying is crushed with micronizer, 1000 mesh screens is crossed, obtains pretreated stalk；
The pretreated stalk yield is greater than 87%；
Pretreated stalk: being added the acetum of pH=3 by the S2. preparation of flexible screen bright enhancement film substrate, using super
Sound wave cell crushing instrument, continuous ultrasound 1-2h under ice bath environment, after ultrasonic treatment, centrifugation takes supernatant, by supernatant spend from
Sub- water dilutes 10 times, is transferred in glass dish, is evaporated moisture under 100 DEG C of water-baths, obtains basement membrane, membrane surface is immersed in second
10-30min in aldehyde and silane coupler solution takes out, and surface uniformly coats silver ammino solution, dries 2-3h at room temperature, obtains soft
Property screen bright enhancement film substrate.
As further improvement of the invention, the mass volume ratio of straw powder described in step S1 and aminotriacetic acid is 1:
(10-20)；The straw powder, N, the mass ratio of accelerine, potassium peroxydisulfate and hydrogen peroxide are 100:(0.1-1):
(0.1-10): (0.1-1).
Improved as of the invention further, the heavy metal chelant be selected from one of HCMA, RDTC and TPEN or
Several mixing.
As further improvement of the invention, ultrasonic power described in step S2 is 800-1000W；The centrifugal rotational speed is
10000-15000rpm, centrifugation time 10-30min, centrifuging temperature are 0-10 DEG C.
It is further improved as of the invention, the quality hundred of acetaldehyde in acetaldehyde described in step S2 and silane coupler solution
Dividing specific concentration is 30-50%, and the mass percent of silane coupling agent is 1-3%；The substance withdrawl syndrome of the silver ammino solution is
3-5mol/L。
The present invention further protects a kind of flexible screen bright enhancement film substrate as made from above-mentioned preparation method, the flexible screen
The tensile strength of bright enhancement film substrate is not less than 395MPa, and dielectric constant is not higher than 2.9.
The present invention further protects a kind of preparation method of flexible screen bright enhancement film substrate, comprising the following steps:
S1. the pretreatment of stalk: dry stalk is crushed with micronizer, obtains straw powder, dry to constant weight, is added
Enter aminotriacetic acid, n,N-Dimethylaniline, potassium peroxydisulfate, hydrogen peroxide, normal-temperature continuous stirs 10-12h, product filtering, filter
Slag is washed with water to neutrality, soluble in water, and heavy metal chelant is added, is stirred to react 2-5h, filters, filtrate decompression evaporation, vacuum
It is dry；Powder after drying is crushed with micronizer, 1000 mesh screens is crossed, obtains pretreated stalk；
The pretreated stalk yield is greater than 90%；
Pretreated stalk: being added the acetum of pH=3 by the S2. preparation of flexible screen bright enhancement film substrate, using super
Sound wave cell crushing instrument, continuous ultrasound 1-2h under ice bath environment, after ultrasonic treatment, centrifugation takes supernatant, by supernatant spend from
Sub- water dilutes 10 times, is transferred in glass dish, is evaporated moisture under 100 DEG C of water-baths, obtains basement membrane, phosphotungstic acid is dissolved in deionization
In water, Salkowski's solution is obtained, is evenly applied to membrane surface, 2-3h is dried at room temperature, obtains flexible screen bright enhancement film substrate.
Improved as of the invention further, the heavy metal chelant be selected from one of HCMA, RDTC and TPEN or
Several mixing.
As further improvement of the invention, ultrasonic power described in step S2 is 800-1000W；The centrifugal rotational speed is
10000-15000rpm, centrifugation time 10-30min, centrifuging temperature are 0-10 DEG C；The pretreated stalk and acetic acid are molten
The mass volume ratio of liquid is 1:(30-70)；The mass percent concentration of the Salkowski's solution is 35-55%.
The present invention further protects a kind of flexible screen bright enhancement film substrate as made from above-mentioned preparation method, and the flexible screen increases
The tensile strength of light film substrate is not less than 402MPa, and dielectric constant is not higher than 3.
The invention has the following beneficial effects:
For the present invention using stalk as raw material, the Performances of Novel Nano-Porous meter level obtained after the processing of specific physico-chemical method Jing Guo chemical modification is fine
Chlorins compound is tieed up, the heavy metal ion adsorbed removal contained by heavy metal chelant obtains the higher fiber of purity
Flexible screen bright enhancement film substrate is being prepared, on conductive and mechanical properties in chlorins compound after coating film formation process
There is great raising.Basement membrane is immersed in acetaldehyde solution, under the action of silane coupling agent, surface is evenly distributed with acetaldehyde point
Son coats silver ammino solution, generates silverskin in membrane surface immediate response, the silverskin is very thin, by improving carrier density and drop
Low contact resistance improves electric conductivity, while there is the flexible screen bright enhancement film substrate to have good mechanical property；
The present invention is also prepared for one kind using stalk as raw material, inhales by the heavy metal ion that heavy metal chelant is contained
Attached removal obtains the higher cellulose compound of purity, after coating film formation process, the diaphragm of squilla oratoria is made soft
Property basement membrane, coat conductive Salkowski's solution allows phosphotungstic acid to be voluntarily aggregated on basement membrane by electrostatic interaction and hydrogen bond, improves base
Film conductivity does not influence the mechanical property of basement membrane simultaneously；
Preparation method of the present invention is simple, raw material sources are wide, at low cost, and nonconducting stalk is made into mechanical property and electricity
The very excellent flexible screen bright enhancement film substrate of performance, while agricultural wastes can be recycled, it is environmentally protective, improve waste utilization
Rate has a vast market foreground.
Detailed description of the invention
Fig. 1 is each experimental group mechanical property comparison diagram in test case 1 of the present invention；
Fig. 2 is each experimental group electric property comparison diagram in test case 1 of the present invention；
Fig. 3 is each experimental group mechanical property comparison diagram in test case 2 of the present invention；
Fig. 4 is each experimental group electric property comparison diagram in test case 2 of the present invention.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, the embodiment described is the embodiment of part of representative of the invention, rather than whole embodiments, this field are general
Other all embodiments obtained belong to protection of the invention to logical technical staff without making creative work
Range.
Embodiment 1
A kind of preparation method of flexible screen bright enhancement film substrate, which comprises the following steps:
S1. the pretreatment of stalk: dry stalk is crushed with micronizer, acquisition straw powder 1g, drying to constant weight,
10mL aminotriacetic acid, 0.001g n,N-Dimethylaniline, 0.001g potassium peroxydisulfate, 0.001g hydrogen peroxide is added, room temperature connects
Continuous stirring 10h, product filtering, filter residue is washed with water to neutrality, soluble in water, and heavy metal chelant HCMA is added, is stirred to react 2h,
Filtering, filtrate decompression evaporation, vacuum drying；Powder after drying is crushed with micronizer, 1000 mesh screens is crossed, obtains pre-
Treated stalk；
The pretreated stalk yield 87%；
Pretreated stalk: being added the acetum of pH=3 by the S2. preparation of flexible screen bright enhancement film substrate, using super
Sound wave cell crushing instrument, continuous ultrasound 1h under ice bath environment, after 800W ultrasonic treatment, 0 DEG C, 10000rpm is centrifuged 10min, takes
Supernatant deionized water is diluted 10 times, is transferred in glass dish, is evaporated moisture under 100 DEG C of water-baths, obtains base by clear liquid
Film, membrane surface is immersed in acetaldehyde and silane coupler solution, and (mass percent concentration of acetaldehyde is 30%, silane coupling agent
Mass percent be 1%) in 10min, take out, surface uniformly coats 3mol/L silver ammino solution, dries 2h at room temperature, obtains soft
Property screen bright enhancement film substrate, yield 95%.
Embodiment 2
A kind of preparation method of flexible screen bright enhancement film substrate, which comprises the following steps:
S1. the pretreatment of stalk: dry stalk is crushed with micronizer, acquisition straw powder 1g, drying to constant weight,
20mL aminotriacetic acid, 0.01g n,N-Dimethylaniline, 0.01g potassium peroxydisulfate, 0.01g hydrogen peroxide, normal-temperature continuous is added
12h is stirred, product filtering, filter residue is washed with water to neutrality, and it is soluble in water, heavy metal chelant RDTC is added, is stirred to react 5h, mistake
Filter, filtrate decompression evaporation, vacuum drying；Powder after drying is crushed with micronizer, 1000 mesh screens is crossed, obtains pre- place
Stalk after reason；
The pretreated stalk yield is 92%；
Pretreated stalk: being added the acetum of pH=3 by the S2. preparation of flexible screen bright enhancement film substrate, using super
Sound wave cell crushing instrument, continuous ultrasound 2h under ice bath environment, after 1000W ultrasonic treatment, 10 DEG C, 15000rpm is centrifuged 30min, takes
Supernatant deionized water is diluted 10 times, is transferred in glass dish, is evaporated moisture under 100 DEG C of water-baths, obtains base by supernatant
Film, membrane surface is immersed in acetaldehyde and silane coupler solution, and (mass percent concentration of acetaldehyde is 50%, silane coupling agent
Mass percent be 3%) in 30min, take out, surface uniformly coats 5mol/L silver ammino solution, dries 3h at room temperature, obtains soft
Property screen bright enhancement film substrate, yield 97%.
Embodiment 3
A kind of preparation method of flexible screen bright enhancement film substrate, which comprises the following steps:
S1. the pretreatment of stalk: dry stalk is crushed with micronizer, acquisition straw powder 1g, drying to constant weight,
15mL aminotriacetic acid, 0.005g n,N-Dimethylaniline, 0.005g potassium peroxydisulfate, 0.005g hydrogen peroxide is added, room temperature connects
Continuous stirring 11h, product filtering, filter residue is washed with water to neutrality, soluble in water, and heavy metal chelant TPEN is added, is stirred to react 3h,
Filtering, filtrate decompression evaporation, vacuum drying；Powder after drying is crushed with micronizer, 1000 mesh screens is crossed, obtains pre-
Treated stalk；
The pretreated stalk yield is 92%；
The pretreated stalk of 1g: being added the acetum of 50mL pH=3 by the S2. preparation of flexible screen bright enhancement film substrate,
Using ultrasonic cell disruption instrument, continuous ultrasound 1.5h under ice bath environment, after 900W ultrasonic treatment, 5 DEG C, 12500rpm centrifugation
20min takes supernatant, and supernatant deionized water is diluted 10 times, is transferred in glass dish, steams moisture under 100 DEG C of water-baths
It is dry, obtain basement membrane, by membrane surface be immersed in acetaldehyde and silane coupler solution (mass percent concentration of acetaldehyde is 40%,
The mass percent of silane coupling agent be 2%) in 20min, take out, surface uniformly coats 4mol/L silver ammino solution, does at room temperature
Dry 2.5h obtains flexible screen bright enhancement film substrate, yield 98%.
Embodiment 4
A kind of preparation method of flexible screen bright enhancement film substrate, comprising the following steps:
S1. the pretreatment of stalk: dry stalk is crushed with micronizer, acquisition straw powder 1g, drying to constant weight,
10mL aminotriacetic acid, 0.001g n,N-Dimethylaniline, 0.001g potassium peroxydisulfate, 0.001g hydrogen peroxide is added, room temperature connects
Continuous stirring 10h, product filtering, filter residue is washed with water to neutrality, soluble in water, and heavy metal chelant HCMA is added, is stirred to react 2h,
Filtering, filtrate decompression evaporation, vacuum drying；Powder after drying is crushed with micronizer, 1000 mesh screens is crossed, obtains pre-
Treated stalk；
The pretreated stalk yield 90%；
The pretreated stalk of 1g: being added the acetum of 30mL pH=3 by the S2. preparation of flexible screen bright enhancement film substrate,
Using ultrasonic cell disruption instrument, continuous ultrasound 1h under ice bath environment, after 800W ultrasonic treatment, 0 DEG C, 10000rpm centrifugation
10min takes supernatant, and supernatant deionized water is diluted 10 times, is transferred in glass dish, steams moisture under 100 DEG C of water-baths
It is dry, basement membrane is obtained, phosphotungstic acid is dissolved in deionized water, obtains 35wt% Salkowski's solution, is evenly applied to membrane surface, room
The lower dry 2h of temperature, obtains flexible screen bright enhancement film substrate, yield 92%.
Embodiment 5
A kind of preparation method of flexible screen bright enhancement film substrate, comprising the following steps:
S1. the pretreatment of stalk: dry stalk is crushed with micronizer, acquisition straw powder 1g, drying to constant weight,
20mL aminotriacetic acid, 0.01g n,N-Dimethylaniline, 0.01g potassium peroxydisulfate, 0.01g hydrogen peroxide, normal-temperature continuous is added
12h is stirred, product filtering, filter residue is washed with water to neutrality, and it is soluble in water, heavy metal chelant RDTC is added, is stirred to react 5h, mistake
Filter, filtrate decompression evaporation, vacuum drying；Powder after drying is crushed with micronizer, 1000 mesh screens is crossed, obtains pre- place
Stalk after reason；
The pretreated stalk yield 92%；
The pretreated stalk of 1g: being added the acetum of 70mL pH=3 by the S2. preparation of flexible screen bright enhancement film substrate,
Using ultrasonic cell disruption instrument, continuous ultrasound 2h under ice bath environment, after 1000W ultrasonic treatment, 10 DEG C, 15000rpm centrifugation
30min takes supernatant, and supernatant deionized water is diluted 10 times, is transferred in glass dish, steams moisture under 100 DEG C of water-baths
It is dry, basement membrane is obtained, phosphotungstic acid is dissolved in deionized water, obtains 55wt% Salkowski's solution, is evenly applied to membrane surface, room
The lower dry 3h of temperature, obtains flexible screen bright enhancement film substrate, yield 95%.
Embodiment 6
A kind of preparation method of flexible screen bright enhancement film substrate, comprising the following steps:
S1. the pretreatment of stalk: dry stalk is crushed with micronizer, acquisition straw powder 1g, drying to constant weight,
15mL aminotriacetic acid, 0.005g n,N-Dimethylaniline, 0.005g potassium peroxydisulfate, 0.005g hydrogen peroxide is added, room temperature connects
Continuous stirring 11h, product filtering, filter residue is washed with water to neutrality, soluble in water, and heavy metal chelant TPEN is added, is stirred to react 3h,
Filtering, filtrate decompression evaporation, vacuum drying；Powder after drying is crushed with micronizer, 1000 mesh screens is crossed, obtains pre-
Treated stalk；
The pretreated stalk yield 95%；
The pretreated stalk of 1g: being added the acetum of 50mL pH=3 by the S2. preparation of flexible screen bright enhancement film substrate,
Using ultrasonic cell disruption instrument, continuous ultrasound 1.5h under ice bath environment, after 900W ultrasonic treatment, 5 DEG C, 12500rpm centrifugation
20min takes supernatant, and supernatant deionized water is diluted 10 times, is transferred in glass dish, steams moisture under 100 DEG C of water-baths
It is dry, basement membrane is obtained, phosphotungstic acid is dissolved in deionized water, obtains 45wt% Salkowski's solution, is evenly applied to membrane surface, room
The lower dry 2.5h of temperature, obtains flexible screen bright enhancement film substrate, yield 97%.
Comparative example 1
A kind of preparation method of flexible screen bright enhancement film substrate, which comprises the following steps:
S1. the pretreatment of stalk: dry stalk is crushed with micronizer, obtains straw powder 10g, dry to perseverance
15mL aminotriacetic acid, 1g n,N-Dimethylaniline, 1g potassium peroxydisulfate, 1g hydrogen peroxide, normal-temperature continuous stirring is added in weight
11h, product filtering, filter residue is washed with water to neutrality, soluble in water, and heavy metal chelant TPEN is added, is stirred to react 3h, filters,
Filtrate decompression evaporation, vacuum drying；Powder after drying is crushed with micronizer, 1000 mesh screens is crossed, is pre-processed
Stalk afterwards；
The pretreated stalk yield is 62%；
S2. the preparation of flexible screen bright enhancement film substrate: the acetic acid that 50mL pH=3 is added in the pretreated stalk of 10g is molten
Liquid, using ultrasonic cell disruption instrument, continuous ultrasound 1.5h under ice bath environment, after 900W ultrasonic treatment, 5 DEG C, 5000rpm centrifugation
5min takes supernatant, and supernatant deionized water is diluted 10 times, is transferred in glass dish, steams moisture under 100 DEG C of water-baths
It is dry, obtain basement membrane, by membrane surface be immersed in acetaldehyde and silane coupler solution (mass percent concentration of acetaldehyde is 40%,
The mass percent of silane coupling agent be 2%) in 20min, take out, surface uniformly coats 4mol/L silver ammino solution, does at room temperature
Dry 2.5h obtains flexible screen bright enhancement film substrate, yield 53%.
Comparative example 2
A kind of preparation method of flexible screen bright enhancement film substrate, which comprises the following steps:
S1. the pretreatment of stalk: dry stalk is crushed with micronizer, acquisition straw powder 1g, drying to constant weight,
15mL aminotriacetic acid, 0.005g n,N-Dimethylaniline, 0.005g potassium peroxydisulfate, 0.005g hydrogen peroxide is added, room temperature connects
Continuous stirring 11h, product filtering, filter residue is washed with water to neutrality, soluble in water, and heavy metal chelant TPEN is added, is stirred to react 3h,
Filtering, filtrate decompression evaporation, vacuum drying；Powder after drying is crushed with micronizer, 1000 mesh screens is crossed, obtains pre-
Treated stalk；
The pretreated stalk yield is 92%；
The pretreated stalk of 1g: being added the acetum of 50mL pH=3 by the S2. preparation of flexible screen bright enhancement film substrate,
Using ultrasonic cell disruption instrument, continuous ultrasound 1.5h under ice bath environment, after 900W ultrasonic treatment, 5 DEG C, 12500rpm centrifugation
20min takes supernatant, and supernatant deionized water is diluted 10 times, is transferred in glass dish, steams moisture under 100 DEG C of water-baths
It is dry, obtain basement membrane, yield 99%.
Comparative example 3
A kind of preparation method of flexible screen bright enhancement film substrate, which comprises the following steps:
S1. the pretreatment of stalk: dry stalk is crushed with micronizer, acquisition straw powder 1g, drying to constant weight,
15mL aminotriacetic acid, 0.005g n,N-Dimethylaniline, 0.005g potassium peroxydisulfate, 0.005g hydrogen peroxide is added, room temperature connects
Continuous stirring 11h, product filtering, filter residue are washed with water to neutrality, vacuum drying；Powder after drying is crushed with micronizer,
1000 mesh screens are crossed, pretreated stalk is obtained；
The pretreated stalk yield is 93%；
The pretreated stalk of 1g: being added the acetum of 50mL pH=3 by the S2. preparation of flexible screen bright enhancement film substrate,
Using ultrasonic cell disruption instrument, continuous ultrasound 1.5h under ice bath environment, after 900W ultrasonic treatment, 5 DEG C, 12500rpm centrifugation
20min takes supernatant, and supernatant deionized water is diluted 10 times, is transferred in glass dish, steams moisture under 100 DEG C of water-baths
It is dry, obtain basement membrane, yield 69%.
Comparative example 4
A kind of preparation method of flexible screen bright enhancement film substrate, comprising the following steps:
S1. the pretreatment of stalk: dry stalk is crushed with micronizer, acquisition straw powder 1g, drying to constant weight,
15mL aminotriacetic acid, 0.005g n,N-Dimethylaniline, 0.005g potassium peroxydisulfate, 0.005g hydrogen peroxide is added, room temperature connects
Continuous stirring 11h, product filtering, filter residue is washed with water to neutrality, soluble in water, and heavy metal chelant TPEN is added, is stirred to react 3h,
Filtering, filtrate decompression evaporation, vacuum drying；Powder after drying is crushed with micronizer, 1000 mesh screens is crossed, obtains pre-
Treated stalk；
The pretreated stalk yield 95%；
The pretreated stalk of 1g: being added the acetum of 50mL pH=3 by the S2. preparation of flexible screen bright enhancement film substrate,
Using ultrasonic cell disruption instrument, continuous ultrasound 1.5h under ice bath environment, after 900W ultrasonic treatment, 5 DEG C, 12500rpm centrifugation
20min takes supernatant, and supernatant deionized water is diluted 10 times, is transferred in glass dish, steams moisture under 100 DEG C of water-baths
It is dry, obtain basement membrane, yield 98%.
Comparative example 5
A kind of preparation method of flexible screen bright enhancement film substrate, comprising the following steps:
S1. the pretreatment of stalk: dry stalk is crushed with micronizer, acquisition straw powder 1g, drying to constant weight,
15mL aminotriacetic acid, 0.005g n,N-Dimethylaniline, 0.005g potassium peroxydisulfate, 0.005g hydrogen peroxide is added, room temperature connects
Continuous stirring 11h, product filtering, filter residue are washed with water to neutrality, vacuum drying；Powder after drying is crushed with micronizer,
1000 mesh screens are crossed, pretreated stalk is obtained；
The pretreated stalk yield 75%；
The pretreated stalk of 1g: being added the acetum of 50mL pH=3 by the S2. preparation of flexible screen bright enhancement film substrate,
Using ultrasonic cell disruption instrument, continuous ultrasound 1.5h under ice bath environment, after 900W ultrasonic treatment, 5 DEG C, 12500rpm centrifugation
20min takes supernatant, and supernatant deionized water is diluted 10 times, is transferred in glass dish, steams moisture under 100 DEG C of water-baths
It is dry, basement membrane is obtained, phosphotungstic acid is dissolved in deionized water, obtains 45wt% Salkowski's solution, is evenly applied to membrane surface, room
The lower dry 2.5h of temperature, obtains flexible screen bright enhancement film substrate, yield 62%.
Test case 1
1-3 of the embodiment of the present invention and comparative example 1-3 flexible screen bright enhancement film substrate prepared and commercial like product are carried out
Performance test, the result is shown in Figure 1 and 2.Annotate in Fig. 1: a is p < 0.05 compared with commercial product；B be compared with commercial product, p <
0.05.Annotate in Fig. 2: * is p < 0.05 compared with commercial product.
It is obtained by Fig. 1, the flexible screen bright enhancement film substrate of 1-3 of embodiment of the present invention preparation is compared to comparative example and commercially available same
Class product has preferable mechanical property.Compared with Example 3, raw material is although identical for comparative example 1, but the concentration of raw material and
Proportion is different, and as shown in Figure 1, mechanical property is greatly reduced comparative example 1 compared with Example 3.Comparative example 2 is not molten using silver-colored ammonia
Liquid, acetaldehyde and coupling agent coat basement membrane, and surface does not generate silverskin, goes after the stalk processing of comparative example 3 without metal-chelator
Except plants enriched heavy metal ion, though flexible screen bright enhancement film substrate mechanical property made from the two is slightly decreased than embodiment 3,
But decline is unobvious, is still apparently higher than commercial like product and comparative example 1.
It is obtained by Fig. 2, the flexible screen bright enhancement film substrate of 1-3 of embodiment of the present invention preparation is compared to comparative example and commercially available same
Class product has preferable electric property.Compared with Example 3, raw material is although identical for comparative example 1, but the concentration of raw material and
Proportion is different, and electric property is greatly reduced, and dielectric constant is very high；Comparative example 2 is not using silver ammino solution, acetaldehyde and coupling agent coating
Basement membrane, surface do not generate silverskin, carrier density decline, and contact resistance improves, and electric property is greatly reduced；Comparative example 3
Plants enriched heavy metal ion is removed without metal-chelator after stalk processing, dielectric constant significantly improves.
Test case 2
4-6 of the embodiment of the present invention and comparative example 4-5 flexible screen bright enhancement film substrate prepared and commercial like product are carried out
As a result performance test is seen figures 3 and 4.Annotate in Fig. 3: a is p < 0.05 compared with commercial product；B be compared with commercial product, p <
0.05.Annotate in Fig. 4: * is p < 0.05 compared with commercial product.
It is obtained by Fig. 3, the flexible screen bright enhancement film substrate of 4-6 of embodiment of the present invention preparation is compared to comparative example and commercially available same
Class product has preferable mechanical property.Comparative example 4 does not coat basement membrane using Salkowski's solution, after the stalk processing of comparative example 5
Plants enriched heavy metal ion is removed without metal-chelator, though flexible screen bright enhancement film substrate mechanical property made from the two
It is slightly decreased than embodiment 3, but decline is unobvious, is still apparently higher than commercial like product.
It is obtained by Fig. 4, the flexible screen bright enhancement film substrate of 1-3 of embodiment of the present invention preparation is compared to comparative example and commercially available same
Class product has preferable electric property.Comparative example 4 is not coated using Salkowski's solution, and electric conductivity is greatly reduced, electricity
Performance is also greatly reduced；Plants enriched heavy metal ion is removed without metal-chelator after the stalk processing of comparative example 5, is situated between
Electric constant significantly improves.
Compared with prior art, the present invention is obtained after the processing of specific physico-chemical method and is repaired by chemistry using stalk as raw material
The Performances of Novel Nano-Porous meter level cellulose compound of decorations, the heavy metal ion adsorbed removal that heavy metal chelant is contained obtain
Flexible screen bright enhancement film substrate is being prepared after coating film formation process, is leading for the higher cellulose compound of purity
There is great raising in electricity and mechanical property.Basement membrane is immersed in acetaldehyde solution, under the action of silane coupling agent, surface
It is evenly distributed with acetaldehyde molecule, coats silver ammino solution, generates silverskin in membrane surface immediate response, the silverskin is very thin, passes through raising
Carrier density improves electric conductivity with contact resistance is reduced, while there is the flexible screen bright enhancement film substrate to have good mechanics
Performance；
The present invention is also prepared for one kind using stalk as raw material, inhales by the heavy metal ion that heavy metal chelant is contained
Attached removal obtains the higher cellulose compound of purity, after coating film formation process, the diaphragm of squilla oratoria is made soft
Property basement membrane, coat conductive Salkowski's solution allows phosphotungstic acid to be voluntarily aggregated on basement membrane by electrostatic interaction and hydrogen bond, improves base
Film conductivity does not influence the mechanical property of basement membrane simultaneously；
Preparation method of the present invention is simple, raw material sources are wide, at low cost, and nonconducting stalk is made into mechanical property and electricity
The very excellent flexible screen bright enhancement film substrate of performance, while agricultural wastes can be recycled, it is environmentally protective, improve waste utilization
Rate has a vast market foreground.
Those skilled in the art is not under conditions of departing from the spirit and scope of the present invention that claims determine, also
Various modifications can be carried out to the above content.Therefore the scope of the present invention is not limited in above explanation, but by
The range of claims determines.
Claims (10)
1. a kind of preparation method of flexible screen bright enhancement film substrate, which comprises the following steps:
S1. the pretreatment of stalk: dry stalk is crushed with micronizer, obtains straw powder, dry to constant weight, and ammonia is added
Base triacetic acid, n,N-Dimethylaniline, potassium peroxydisulfate, hydrogen peroxide, normal-temperature continuous stir 10-12h, product filtering, and filter residue is used
It is washed to neutrality, it is soluble in water, heavy metal chelant is added, is stirred to react 2-5h, filters, filtrate decompression evaporation, vacuum drying；
Powder after drying is crushed with micronizer, 1000 mesh screens is crossed, obtains pretreated stalk；
The pretreated stalk yield is greater than 87%；
S2. the preparation of flexible screen bright enhancement film substrate: pretreated stalk is added to the acetum of pH=3, uses ultrasonic wave
Cell crushing instrument, continuous ultrasound 1-2h under ice bath environment, after ultrasonic treatment, centrifugation takes supernatant, by supernatant deionized water
Dilution 10 times, be transferred in glass dish, moisture be evaporated under 100 DEG C of water-baths, obtains basement membrane, by membrane surface be immersed in acetaldehyde and
10-30min in silane coupler solution takes out, and surface uniformly coats silver ammino solution, dries 2-3h at room temperature, obtains flexible screen
Bright enhancement film substrate.
2. a kind of preparation method of flexible screen bright enhancement film substrate according to claim 1, which is characterized in that described in step S1
The mass volume ratio of straw powder and aminotriacetic acid is 1:(10-20)；The straw powder, N, accelerine, potassium peroxydisulfate
Mass ratio with hydrogen peroxide is 100:(0.1-1): (0.1-10): (0.1-1).
3. a kind of preparation method of flexible screen bright enhancement film substrate according to claim 1, which is characterized in that the heavy metal chela
Mixture is selected from one or more of HCMA, RDTC and TPEN mixing.
4. a kind of preparation method of flexible screen bright enhancement film substrate according to claim 1, which is characterized in that described in step S2
Ultrasonic power is 800-1000W；The centrifugal rotational speed is 10000-15000rpm, centrifugation time 10-30min, centrifuging temperature
It is 0-10 DEG C.
5. a kind of preparation method of flexible screen bright enhancement film substrate according to claim 1, which is characterized in that described in step S2
The mass percent concentration of acetaldehyde is 30-50% in acetaldehyde and silane coupler solution, and the mass percent of silane coupling agent is
1-3%；The substance withdrawl syndrome of the silver ammino solution is 3-5mol/L.
6. flexible screen bright enhancement film substrate made from a kind of preparation method as described in any one of claim 1-5 claim, special
Sign is that the tensile strength of the flexible screen bright enhancement film substrate is not less than 395MPa, and dielectric constant is not higher than 2.9.
7. a kind of preparation method of flexible screen bright enhancement film substrate, which comprises the following steps:
S1. the pretreatment of stalk: dry stalk is crushed with micronizer, obtains straw powder, dry to constant weight, and ammonia is added
Base triacetic acid, n,N-Dimethylaniline, potassium peroxydisulfate, hydrogen peroxide, normal-temperature continuous stir 10-12h, product filtering, and filter residue is used
It is washed to neutrality, it is soluble in water, heavy metal chelant is added, is stirred to react 2-5h, filters, filtrate decompression evaporation, vacuum drying；
Powder after drying is crushed with micronizer, 1000 mesh screens is crossed, obtains pretreated stalk；
The pretreated stalk yield is greater than 90%；
S2. the preparation of flexible screen bright enhancement film substrate: pretreated stalk is added to the acetum of pH=3, uses ultrasonic wave
Cell crushing instrument, continuous ultrasound 1-2h under ice bath environment, after ultrasonic treatment, centrifugation takes supernatant, by supernatant deionized water
10 times of dilution, is transferred in glass dish, is evaporated moisture under 100 DEG C of water-baths, obtains basement membrane, phosphotungstic acid is dissolved in deionized water
In, Salkowski's solution is obtained, membrane surface is evenly applied to, 2-3h is dried at room temperature, obtains flexible screen bright enhancement film substrate.
8. a kind of preparation method of flexible screen bright enhancement film substrate according to claim 7, which is characterized in that the heavy metal chela
Mixture is selected from one or more of HCMA, RDTC and TPEN mixing.
9. a kind of preparation method of flexible screen bright enhancement film substrate according to claim 7, which is characterized in that described in step S2
Ultrasonic power is 800-1000W；The centrifugal rotational speed is 10000-15000rpm, centrifugation time 10-30min, centrifuging temperature
It is 0-10 DEG C；The mass volume ratio of the pretreated stalk and acetum is 1:(30-70)；The Salkowski's solution
Mass percent concentration is 35-55%.
10. flexible screen bright enhancement film substrate made from a kind of preparation method as described in any one of claim 7-9 claim, special
Sign is that the tensile strength of the flexible screen bright enhancement film substrate is not less than 402MPa, and dielectric constant is not higher than 3.
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