CN107134542A - Transparent single-side coated copper plate manufacture craft - Google Patents
Transparent single-side coated copper plate manufacture craft Download PDFInfo
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- CN107134542A CN107134542A CN201710229698.8A CN201710229698A CN107134542A CN 107134542 A CN107134542 A CN 107134542A CN 201710229698 A CN201710229698 A CN 201710229698A CN 107134542 A CN107134542 A CN 107134542A
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- coated copper
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1003—Preparatory processes
- C08G73/1007—Preparatory processes from tetracarboxylic acids or derivatives and diamines
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1067—Wholly aromatic polyimides, i.e. having both tetracarboxylic and diamino moieties aromatically bound
- C08G73/1071—Wholly aromatic polyimides containing oxygen in the form of ether bonds in the main chain
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K77/00—Constructional details of devices covered by this subclass and not covered by groups H10K10/80, H10K30/80, H10K50/80 or H10K59/80
- H10K77/10—Substrates, e.g. flexible substrates
- H10K77/111—Flexible substrates
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
The present invention proposes a kind of transparent single-side coated copper plate manufacture craft, and raw material includes copper foil and hyaline layer, and this product hyaline layer is polyimides, and processing step is：One, produce polyimide solution；Two, polyimide solution is coated on the copper foil by coating machine；Three, it is cured as finished product.The present invention is by using dimethyl acetamide, p-phenylenediamine, 4,4 ' diaminodiphenyl ethers (ODA) carry out copolyreaction to reach the Kapton of high transparency with bibenzene tetracarboxylic dianhydride, water white transparency single-side coated copper plate is made in collocation coating technique, it will be expected to that the core material glass for being currently used for display can be replaced, and promote developing rapidly for photovoltaic industry.
Description
Technical field
Field is manufactured the present invention relates to copper-clad plate, a kind of transparent single-side coated copper plate manufacture craft is particularly related to.
Background technology
Research and development of the China to polyimides are started from 1962, and enamel-covered wire comes out within 1963, rear film, molding in 1966
Material, adhesive are come out one after another.Up to the present, research and development form rational general layout, Changchun applied chemistry study so poly- connection
Based on the research and development of diimides, Chinese Academy of Sciences's chemistry specializes in the research and development of PMR polyimides, Sichuan joint
University (Chengdu Univ. of Science ＆ Technology), research bimaleimide resin and product, Northwestern Polytechnical University is ground with polyamidoimide
Study carefully based on exploitation, SHANGHAI RESEARCH INSTITUTE OF SYNTHETIC RESINS is to research and develop PMMI, based on PEI, Guilin
Electrical science research institute is to research and develop based on the casting device of Kapton.According to incompletely statistics, polyimides is ground
Study carefully development and application unit family about more than 50, mainly research and produce producer about 20；Production development has begun to take shape, and the whole nation is raw at present
Production capacity power reaches 700t/a, with the development of China's Aeronautics and Astronautics, electrical equipment, electronics industry and auto industry, polyimides industry
Also big development is had.
Clear polyimides (PI) were developed in Korea S's Cologne industry in 2016, OLED were mainly used in, because PI possesses
The characteristic that can be destroyed or force to yield, was once used on deflection screen mobile phone, so to transmit the color of deflection display, transparent material
It is indispensable.In addition to Korea S's Cologne industry, TaiWan, China is up to the science and technology also transparent PI of active development is stepped, because transparent PI is by market
Think most to be hopeful substitution display core material-glass.
With the evolution of secondary generation display, the glass higher compared to hardness, the transparent PI of deflection starts by weight
Depending on, therefore keeping being modified Develop new product in the original characteristic of polyimides, will to improve the translucency of Kapton
It is the developing focus of prospective material manufacturer.
The polyimides of high transparency is one of hot research topic in functional polyalkylene acid imide investigation of materials field.Nothing
Color transparency PI materials are respectively provided with many high-tech sectors to be widely applied, such as is used to make in optical-fibre communications field
Optical waveguide；It is used as baseplate material and antenna-reflected/collector material of solar battery array etc. in aerospace field.
By taking the deflection screen mobile phone of recent cell phone manufacturer's active development as an example, deflection display is used, in display medial and lateral
It is able to will must be imaged；In other words, the both sides up and down by substrate, but institute so far be must be able to from the OLED light released
The PI used, can not can not all transmit primary colors, because traditional polyimides membrane material is difficult to accomplish high transparency, with the equal acid anhydride of benzene four
The polyimides synthesized with 4,4'- diphenyldiamines, it is seen that light absorbs end extends to 500nm or so, color be all yellowish-brown or
Dark brown.
The content of the invention
The present invention proposes a kind of transparent single-side coated copper plate manufacture craft, solves the problems of the prior art.
The technical proposal of the invention is realized in this way：
Transparent single-side coated copper plate manufacture craft, raw material includes copper foil and hyaline layer, and this product hyaline layer is polyimides, work
Skill step is：One, produce polyimide solution；Two, polyimide solution is coated on the copper foil by coating machine；Three,
It is cured as finished product.
As the preferred scheme of the present invention, the copper foil is low roughness copper foil, its roughness Rz≤1 μm.
As the preferred scheme of the present invention, producing polyimide solution step includes：One, produce stoste；Two, solid content is adjusted
Section；Three, vacuum defoamation；Four, filtering.
As the preferred scheme of the present invention, polyamic acid stoste is by dimethyl acetamide, p-phenylenediamine, 4,4 '-diaminourea
Diphenyl ether is polymerized with bibenzene tetracarboxylic dianhydride, and polymerization process is by the way of low temperature rubber alloy.
As the preferred scheme of the present invention, stoste each component mass ratio is：Dimethyl acetamide 350ml~450ml is right
1.1~1.3mol of phenylenediamine；4,4 '-diaminodiphenyl ether biphenyl, 1.1~1.3mol；Above-mentioned material is mixed after 30min, plus
Enter 0.8~1.1mol of bibenzene tetracarboxylic dianhydride, continue to stir until sticky.
As the preferred scheme of the present invention, in solid content regulating step, into stoste, addition dimethyl acetamide makes original
Fluid solid content reaches 20%.
As the preferred scheme of the present invention, reach that the viscous fluid of solid content stands 30min~60min under 10 DEG C of environment
Afterwards, persistently stirring 24h obtains colourless viscous fluid of polyamide acid.
As the preferred scheme of the present invention, filtration step is filtered using 5um Teflon filters, is filtrated to get surface viscosity
For 20000-30000CPS viscous fluid.
As the preferred scheme of the present invention, it is cured as finished product step to be put into the copper foil for having coated viscous fluid of polyamide acid
Toasted in baking oven, temperature is 120-200 DEG C, and the time is 10min-60min.
As the preferred scheme of the present invention, the product after baking is put in cyclisation case and is cyclized, and is filled in the cyclisation case
Inert gas, the cyclisation time is 6h~12h.
Beneficial effect:
The present invention proposes a kind of transparent single-side coated copper plate manufacture craft, and raw material includes copper foil and hyaline layer, and this product is saturating
Bright layer is polyimides, and processing step is：One, produce polyimide solution；Two, polyimide solution is coated by coating machine
In on the copper foil；Three, it is cured as finished product.The present invention is by using dimethyl acetamide, p-phenylenediamine, 4,4 '-diaminourea two
Phenylate (ODA) carries out copolyreaction to reach the Kapton of high transparency, collocation coating skill with bibenzene tetracarboxylic dianhydride
Water white transparency single-side coated copper plate is made in art, will be expected to that the core material glass for being currently used for display can be replaced, and promote light
Electric industry is developed rapidly.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the accompanying drawing used required in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments of invention, for those of ordinary skill in the art, without having to pay creative labor, may be used also
To obtain other accompanying drawings according to these accompanying drawings.
Fig. 1 is schematic structural view of the invention.
In figure, copper foil 1, hyaline layer 2.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based on this
Embodiment in invention, the every other reality that those of ordinary skill in the art are obtained under the premise of creative work is not made
Example is applied, the scope of protection of the invention is belonged to.
As shown in figure 1, transparent single-side coated copper plate manufacture craft, raw material includes copper foil 1 and hyaline layer 2, this product hyaline layer
For polyimides, processing step is：One, produce polyimide solution；Two, polyimide solution is coated on by institute by coating machine
State on copper foil；Three, it is cured as finished product.
Copper foil is low roughness copper foil, its roughness Rz≤1 μm.
Producing polyimide solution step includes：One, produce stoste；Two, solid content regulation；Three, vacuum defoamation；Four, mistake
Filter.
Polyamic acid stoste is by dimethyl acetamide, p-phenylenediamine, 4,4 '-diaminodiphenyl ether and bibenzene tetracarboxylic dianhydride
(BPDA) it is polymerized, polymerization process is by the way of low temperature rubber alloy.
Stoste each component mass ratio is：Dimethyl acetamide 350ml~450ml, 1.1~1.3mol of p-phenylenediamine；4,
4 '-diaminodiphenyl ether biphenyl, 1.1~1.3mol；Above-mentioned material is mixed after 30min, adds bibenzene tetracarboxylic dianhydride 0.8
~1.1mol, continues to stir until sticky.
In solid content regulating step, into stoste, addition dimethyl acetamide makes stoste solid content reach 20%.
Reach that the viscous fluid of solid content is stood after 30min~60min under 10 DEG C of environment, persistently stir 24h and obtain colourless
Viscous fluid of polyamide acid.
Filtration step is filtered using 5um Teflon filters, and it is the viscous of 20000-30000CPS to be filtrated to get surface viscosity
Magma.
It is that the copper foil for having coated viscous fluid of polyamide acid is put into baking oven to toast to be cured as finished product step, and temperature is 120-
200 DEG C, the time is 10min-60min.
Product after baking is put in cyclisation case and is cyclized, filling with inert gas in the cyclisation case, and the cyclisation time is 6h
~12h.
Embodiment 1
The polyamic acid solution is by dimethyl acetamide (DMAC), p-phenylenediamine (PPDA), 4,4 '-diaminodiphenyl ether
(ODA) it is polymerized with bibenzene tetracarboxylic dianhydride (BPDA), polymerization process is by the way of low temperature rubber alloy.Polyamic acid solution
Preparation method is to take to add 400ml dimethyl acetamides (DMAC) in 1000ml bottles, adds 1.2mol1, p-phenylenediamine
(PPDA), 4,4 '-diaminodiphenyl ether (ODA) biphenyl stirs 30min, and dissolving is complete, obtains colourless solution, adds 1mol
Bibenzene tetracarboxylic dianhydride (BPDA)：Stirring, solution is gradually become viscous, and the tune of solid content is carried out with dimethyl acetamide (DMAC)
Section, makes up to 20%.Polymerization process is kept at 10 DEG C, fully makes polymerisation complete.Continue stirring reaction 24h and obtain nothing
Polyamic acid (PAA) viscous fluid of color.PAA viscous fluids are carried out vacuum defoamation, then it is insoluble with the removing of 5um Teflon filters
Thing is then sticky by transparent PAA using coating machine to obtain PAA viscous fluid of the uniform apparent viscosity as 20000-30000CPS
Liquid is coated on copper foil, is toasted at 120-200 DEG C, is waited after baking after its cooling, volume is covered to the single substrate of completion
Place and high temperature cyclization is carried out in baking oven, transparent PI is changed under inert gas shielding.Result of study shows, ultralow roughness copper
Paper tinsel does not produce significant impact to the heat resistance, mechanical property and electrical property of clear polyimides material, but can be with significant
Increase the transparency in visible-range, and with splendid resistance to flexibility.
The key point of the present invention：
(1) new material is arranged in pairs or groups：Ultralow roughness copper foil, Matte Side roughness Rz≤1 μm；
(2) it is formulated designing technique：Using containing 4,4 '-diaminodiphenyl ether (ODA), p-phenylenediamine (PPDA), biphenyl tetracarboxylic
Acid dianhydride (BPDA) and the know-how of dimethyl acetamide (DMAC) are formulated to reduce conjugation and introduce macoradical to carry
Its high transparency, allows Kapton that clear, colorless is presented；
(3) technology of curing：The more stable hot imidization of polyamic acid solution is enable into poly- using ladder-elevating temperature method
Imide membrane；
(4) technology of coating：Using continous way rubbing method, accurate control is carried out to coating；
(5) synthesis technology of glue：Its efficiency is improved with the technological design of semi-finished product, shortens processing time.
The innovative point of the present invention：
1st, closed using dimethyl acetamide (DMAC), p-phenylenediamine (PPDA), 4,4 '-diaminodiphenyl ether (ODA) stirring
Into colourless solution, and add bibenzene tetracarboxylic dianhydride (BPDA) and turn into sour (PAA) solution of transparent polyamide of tool toughness, except
Remove the Kapton that hot imidization is obtained after solvent, you can reach the effect of clear, colorless；
2nd, control of the synthesis to temperature so that the color of glue is more transparent；
3rd, using ultralow roughness copper foil, such as HA-V2 calendering copper, so as to improve the effect of PI translucency；
4th, using the cyclisation equipment full of nitrogen, collocation use ladder-elevating temperature method, can effectively with stably will be saturating on copper foil
Bright polyamic acid solution hot imidization is into transparent polyimide film；
5th, product is made to carry out continuously producing and improving efficiency using coating arts techniques；
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God is with principle, and any modification, equivalent substitution and improvements made etc. should be included in the scope of the protection.
Claims (10)
1. transparent single-side coated copper plate manufacture craft, raw material includes copper foil and hyaline layer, it is characterised in that this product hyaline layer is poly-
Acid imide, processing step is：One, produce polyimide solution；Two, polyimide solution is coated on by the copper by coating machine
On paper tinsel；Three, it is cured as finished product.
2. transparent single-side coated copper plate manufacture craft according to claim 1, it is characterised in that the copper foil is low roughness
Copper foil, its roughness Rz≤1 μm.
3. transparent single-side coated copper plate manufacture craft according to claim 1, it is characterised in that produce polyimide solution step
Suddenly include：One, produce stoste；Two, solid content regulation；Three, vacuum defoamation；Four, filtering.
4. transparent single-side coated copper plate manufacture craft according to claim 3, it is characterised in that polyamic acid stoste is by diformazan
Yl acetamide, p-phenylenediamine, 4,4 '-diaminodiphenyl ether are polymerized with bibenzene tetracarboxylic dianhydride (BPDA), and polymerization process is adopted
With the mode of low temperature rubber alloy.
5. transparent single-side coated copper plate manufacture craft according to claim 4, it is characterised in that stoste each component mass ratio
For：Dimethyl acetamide 350ml~450ml, 1.1~1.3mol of p-phenylenediamine；4,4 '-diaminodiphenyl ether biphenyl 1.1~
1.3mol；Above-mentioned material is mixed after 30min, adds 0.8~1.1mol of bibenzene tetracarboxylic dianhydride, continues to stir until viscous
It is thick.
6. transparent single-side coated copper plate manufacture craft according to claim 3, it is characterised in that in solid content regulating step
In, into stoste, addition dimethyl acetamide makes stoste solid content reach 20%.
7. transparent single-side coated copper plate manufacture craft according to claim 6, it is characterised in that reach the viscous fluid of solid content
Stood under 10 DEG C of environment after 30min~60min, persistently stir 24h and obtain colourless viscous fluid of polyamide acid.
8. transparent single-side coated copper plate manufacture craft according to claim 3, it is characterised in that filtration step is special using 5um
Fluorine dragon filter filtering, is filtrated to get the viscous fluid that surface viscosity is 20000-30000CPS.
9. transparent single-side coated copper plate manufacture craft according to claim 1, it is characterised in that it is to incite somebody to action to be cured as finished product step
The copper foil for having coated viscous fluid of polyamide acid is put into baking in baking oven, and temperature is 120-200 DEG C, and the time is 10min-60min.
10. transparent single-side coated copper plate manufacture craft according to claim 9, it is characterised in that the product after baking is put in
It is cyclized in cyclisation case, filling with inert gas in the cyclisation case, the cyclisation time is 6h~12h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710229698.8A CN107134542A (en) | 2017-04-10 | 2017-04-10 | Transparent single-side coated copper plate manufacture craft |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710229698.8A CN107134542A (en) | 2017-04-10 | 2017-04-10 | Transparent single-side coated copper plate manufacture craft |
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| Publication Number | Publication Date |
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Family
ID=59716809
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| CN201710229698.8A Pending CN107134542A (en) | 2017-04-10 | 2017-04-10 | Transparent single-side coated copper plate manufacture craft |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114437348A (en) * | 2022-03-10 | 2022-05-06 | 长沙道尔顿电子材料有限公司 | Liquid crystal orientation agent and preparation method and application thereof |
| CN115594846A (en) * | 2022-09-14 | 2023-01-13 | 安徽国风新材料股份有限公司（Cn） | Polyimide film having improved adhesive force and moisture permeation rate and method for preparing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114437348A (en) * | 2022-03-10 | 2022-05-06 | 长沙道尔顿电子材料有限公司 | Liquid crystal orientation agent and preparation method and application thereof |
| CN115594846A (en) * | 2022-09-14 | 2023-01-13 | 安徽国风新材料股份有限公司（Cn） | Polyimide film having improved adhesive force and moisture permeation rate and method for preparing the same |
| CN115594846B (en) * | 2022-09-14 | 2024-03-15 | 安徽国风新材料股份有限公司 | Polyimide film with improved adhesion and moisture permeation rate and method of preparing the same |
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Application publication date: 20170905 |