CN102391532A - Biaxially oriented polyimide film for flexible printed circuit board base material and preparation method of biaxially oriented polyimide film - Google Patents
Biaxially oriented polyimide film for flexible printed circuit board base material and preparation method of biaxially oriented polyimide film Download PDFInfo
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- CN102391532A CN102391532A CN 201110248294 CN201110248294A CN102391532A CN 102391532 A CN102391532 A CN 102391532A CN 201110248294 CN201110248294 CN 201110248294 CN 201110248294 A CN201110248294 A CN 201110248294A CN 102391532 A CN102391532 A CN 102391532A
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Abstract
The invention relates to a biaxially oriented polyimide film for flexible printed circuit board base material and a preparation method of the biaxially oriented polyimide film. The method is characterized by mainly comprising the following steps of: (1) polymerizing: preparing a basic solution of polyimide acid according to the following proportions: 1-5% of p-phenylenediamine, 2-8% of biphenyltetracarboxylic dianhydride, 5-10% of diaminodiphenyl ether, 8-15% of pyromellitic dianhydride and 62-84% of dimethylacetylamide; (2) salivating the solution into a film; (3) longitudinally stretching the film according to the stretching ratio of 1:1.02-1.15; (4) transversely stretching the film according to the stretching ratio of 1:1.05-1.2 and carrying out imidization; (5) cutting the edge and rolling up the film; (6) postprocessing the film; and (7) cutting and packaging the film. The special biaxially oriented polyimide film material conforming to the flexible printed circuit board base material can be obtained by using the preparation method provided by the invention.
Description
Technical field
The present invention relates to a kind of Kapton and preparation method thereof, relate in particular to a kind of flexible print wiring board base material, belong to the organic polymer material preparation field with two-way stretch Kapton and preparation method.
Background technology
The producer of domestic production two-way stretch Kapton adopts very primary Technology mostly at present; All adopt the practice of two kinds of a kind of solvents of raw material; Promptly be by pyromellitic acid anhydride (PMDA) and diaminodiphenyl oxide (ODA) in extremely strong property solvent N,N-DIMETHYLACETAMIDE (DMAC) through polycondensation and hydrostomia film forming, form through imidization again.Its finished film rate of producing is low, be used for the flexible print wiring board base material especially seldom, most film is used for flexible print wiring, work-ing life is very short, even can not use.Major defect shows:
1., thickness deviation is big, uneven film thickness is even, the use of influence on flexible sheet.
2., tensile strength is low; Linear expansivity and flexibility coat copper plate differ bigger, and in the time of on being used for flexible sheet, circuit has some temperature rises in use; Because of the tensile strength of film not enough; Linear expansivity and flexibility coat copper plate differ bigger, make the copper cash that etching stays on the circuit card, because of with different damage of expanded by heating amount of film.
3., the stripping strength of film and copper-clad plate is not enough, can not be bonded together securely with flexible copper-clad.
Summary of the invention
One of the object of the invention is to overcome above-mentioned deficiency, provides that a kind of film thickness is even, thickness deviation is little, tensile strength is high, can use the two-way stretch Kapton with the flexible print wiring board base material that flexible copper-clad is bonded together securely.
Two of the object of the invention is to provide the preparation method of a kind of flexible print wiring board base material with the two-way stretch Kapton.
The objective of the invention is to realize like this:
A kind of flexible print wiring board base material is used the two-way stretch Kapton,
Said film is to be specifically designed to the flexible print wiring board base material, and its thickness is 12.75 microns, and thickness deviation is less than ± 0.5mm, apparently is golden yellow.
The tensile strength of said film (vertically) >=200MPa; Tensile strength (laterally) >=210MPa.
The elongation at break 35% ~ 40% of said film; Shrinking percentage≤0.6%; Linear expansivity 40 * 10
-5Electrical strength>=300KV/mm; Thermal weight loss (5%) temperature=510 ℃.
A kind of flexible print wiring board base material is with the preparation method of two-way stretch Kapton, and said method concrete steps are:
(1) polymerization; Carry out the preparation of polyimide acid stoste by following proportioning:
| Ursol D | Bibenzene tetracarboxylic dianhydride | Diaminodiphenyl oxide | Pyromellitic acid anhydride | N,N-DIMETHYLACETAMIDE |
| 1%~5% | 2%~8% | 5%~10% | 8%~15% | 62%~84% |
The stoste of processing is brown transparent colloid, and viscosity is 180PaS ~ 220PaS
(2) hydrostomia film forming; To prepare stoste and carry out deaeration and handle, and after leaving standstill 10 hours, with it with 1.4MPa pressure injection pressure coventry type die head coventry, film forming in slobbering machine then, the speed of travel of slobbering machine is that 4.9m/min ~ 10m/min is adjustable.Temperature regulating range is from 180 ℃ ~ 215 ℃ in the slobbering machine
(3) vertical drawing; The thick film of slobbering machine output enters in the vertical machine drawing, is heated to more than 150 ℃ through preheat roll, carries out 2 stretchings then, and stretch ratio is 1:1.02 ~ 1.15.Derive through 140 ℃ setting roll typing back afterwards.
(4) horizontal drawing and imidization: enter on the transverse stretching machine at once from indulging the film that comes out in the machine drawing; Transverse stretching machine is placed in the imidization stove; Along with the operation of film on transverse stretching machine, film is by cross directional stretch, and stretch ratio is 1:1.05 ~ 1.2 and constantly receives the interior differing temps of stove in heating; Thereby make molecule generation cyclization in the film, slough moisture.Temperature is adjustable to 600 ℃ from 150 ℃ in the stove.In the time of 150 ℃, horizontally draw back the beginning, horizontal drawknot bundle when temperature reaches 600 ℃, is come out of the stove more than the kind through 450 ℃ of temperature typings 1 minute more then.
(5) side cut rolling: with horizontal draw and imidization after the slitter edge on film two limits cut rolling then.
(6) aftertreatment: after film unreeled out, import in 95 ℃ the vaal water groove cleaning and removing foreign material, and the stress that produces because of stretching on the heat abstraction film that adds through water temperature.
(7) cut packing: the film that aftertreatment is accomplished is through cutting machine; Be cut into the wide cut of customer requirement, wrap into tr then, this link is carried out in clean room; Clean degree requirement, the dust granules that surpasses 1 emblem rice that contains in every mark side air must not be above 1000.
A kind of flexible print wiring board base material provided by the invention through selected raw material, formulation optimization and special technology adjustment, is produced the special-purpose two-way stretch Kapton of flexible print wiring board base material with two-way stretch Kapton and preparation method
Use the two-way stretch Kapton of the present invention's preparation, its tensile strength (vertically) >=200MPa; Tensile strength (laterally) >=210MPa.And domestic like product tensile strength generally have only below the 180MPa.
The thickness deviation of film is the important indicator of a quality product, and the two-way stretch Kapton thickness of the present invention preparation is that the apparent of 12.75 microns ± 0.5mm is golden yellow, and state is bigger with general like product thickness deviation, apparently is brown.
A kind of flexible print wiring board base material provided by the invention is with its preparation method of two-way stretch Kapton; Its polymerization stoste has adopted four kinds of a kind of solvents of raw material; The practice that is different from two kinds of a kind of solvents of raw material in the traditional product makes it therefore have better chemical property.
In sum, flexible print wiring board base material of the present invention can obtain to meet the special-purpose two-way stretch polyimide film material of flexible print wiring board base material request for utilization with two-way stretch Kapton and preparation method.
Embodiment
Embodiment 1
Proportioning raw materials in this example is: Ursol D (PDA) 2.78%g, bibenzene tetracarboxylic dianhydride (BPDA) 6%, diaminodiphenyl oxide (ODA) 8%, pyromellitic acid anhydride (PMDA) 12.8%, N,N-DIMETHYLACETAMIDE (DMAC) 70.42%Kg
Above-mentioned raw materials is subsequent use by promptly deciding after the proportion speed weighing.
Load weighted N,N-DIMETHYLACETAMIDE is put in the reaction kettle, added whole Ursol D, mix after 15 minutes; Add load weighted bibenzene tetracarboxylic dianhydride; Stir after 30 minutes, add whole diaminodiphenyl oxides, divide three to four times then while stirring and add pyromellitic acid anhydride.Stirred 3 hours, and carried out deaeration then and handle, reacted stoste was left standstill 10 hours under negative pressure state, the bubble floating in the stoste is deviate from vacuumizing in the jar.
After filtering with pump input slobbering machine die head, input pressure is 1.5MPa with stoste, and stoste extrudes through the die head lip; Be coated on equably on the steel band of slobbering machine; Under the drive of steel band (speed is 6M/min), in the indoor operation of slobbering machine upper and lower cavity, the indoor 200 ℃ of hot blasts that have blower fan to send into of slobbering machine upper and lower cavity; Hot blast is taken the acetic acid dimethylamide of 90% in the film out of, and just one-step forming is laggard goes into vertical machine drawing for final film.
Film at first is heated to more than 150 ℃ through preheat roll after getting into vertical machine drawing, and stretched then roller through two draw roll different speed ratios, makes film obtain longitudinal stretching, and stretch ratio is 1:1.1.
Film through after vertical the drawing enters in the transverse stretching machine, and under the stretch ratio of 1:1.08, the width of film becomes more and more wideer.Transverse stretching machine is placed in the imidization stove, and the quartz glass tube heating source is arranged in the stove, and film horizontally draws back the beginning in the time of 150 ℃, and horizontal drawknot bundle when temperature reaches 600 ℃, is come out of the stove more than the kind through 450 ℃ of temperature typings 1 minute more then.
Through the Kapton of two-way stretch and imidization, its two limit wide slitter edge of 40mm of respectively having an appointment, after it is cut away, the traction rolling.
After film unreeled out, import in 95 ℃ the vaal water groove cleaning and removing foreign material, and the stress that produces because of stretching on the heat abstraction film that adds through water temperature.
The film of finishing dealing with is cut into the wide cut of customer requirement through cutting machine, wraps into tr then, and this link is carried out in clean room, clean degree requirement, and the dust granules that surpasses 1 emblem rice that contains in every mark side air must not be above 1000.
The performance difference of product performance that flexible print wiring board base material of the present invention produces with two-way stretch Kapton and preparation method and general two-way stretch Kapton is asked for an interview down page table:
Can know that through last table the two-way stretch Kapton through the present invention's preparation on the performance of each index such as tensile strength, elongation at break, shrinking percentage, linear expansivity, is superior to common product.Can satisfy the base material that is used for flexible print wiring board fully uses.
Claims (8)
1. a flexible print wiring board base material is with the preparation method of two-way stretch Kapton, and it is characterized in that: said method mainly comprises the steps:
(1) polymerization; Carry out the preparation of polyimide acid stoste by following proportioning: Ursol D 1-5%, bibenzene tetracarboxylic dianhydride 2-8%, diaminodiphenyl oxide 5-10%, pyromellitic acid anhydride 8-15%, N,N-DIMETHYLACETAMIDE 62-84%;
(2) hydrostomia film forming; To prepare stoste and carry out deaeration and handle, and after leaving standstill, with it with 1.4MPa pressure injection pressure coventry type die head coventry, film forming in slobbering machine then;
(3) vertical drawing; The thick film of slobbering machine output enters in the vertical machine drawing, is heated to more than 150 ℃ through preheat roll, carries out 2 stretchings then, and stretch ratio is 1:1.02 ~ 1.15; Derive through 140 ℃ setting roll typing back afterwards;
(4) horizontal drawing and imidization: enter on the transverse stretching machine at once from indulging the film that comes out in the machine drawing; Transverse stretching machine is placed in the imidization stove; Along with the operation of film on transverse stretching machine, film is by cross directional stretch, and stretch ratio is 1:1.05 ~ 1.2 and constantly receives the interior differing temps of stove in heating; Thereby make molecule generation cyclization in the film, slough moisture;
(5) side cut rolling: with horizontal draw and imidization after the slitter edge on film two limits cut rolling then;
(6) aftertreatment: after film unreeled out, cleaning and removing foreign material in the de-ionized tank, and the stress that produces because of stretching on the heat abstraction film that adds through water temperature;
(7) cut packing.
2. a kind of flexible print wiring board base material according to claim 1 is with the preparation method of two-way stretch Kapton; It is characterized in that: the concrete grammar of said step (1) stoste configuration is: earlier load weighted N,N-DIMETHYLACETAMIDE is put in the reaction kettle; Add whole Ursol D, mix after 10-20 minute, add load weighted bibenzene tetracarboxylic dianhydride; Stir after 25-40 minute; Add whole diaminodiphenyl oxides, divide three to four times then while stirring and add pyromellitic acid anhydride, process polyimide acid stoste.
3. a kind of flexible print wiring board base material according to claim 1 is with the preparation method of two-way stretch Kapton; It is characterized in that: in the said step (2); The speed of travel of said slobbering machine is 4.9m/min ~ 10m/min, and temperature regulating range is from 180 ℃ ~ 215 ℃ in the slobbering machine.
4. a kind of flexible print wiring board base material according to claim 1 is with the preparation method of two-way stretch Kapton; It is characterized in that: in the said step (4); In the time of 150 ℃, horizontal beginning, the horizontal drawknot bundle when temperature reaches 600 ℃ of drawing back; Finalize the design 1 fen more than the kind through 450 ℃ of temperature again, come out of the stove then.
5. a kind of flexible print wiring board base material according to claim 1 is characterized in that with the preparation method of two-way stretch Kapton: the vaal water temperature is 90-99 ℃ described in the said step (6).
6. a kind of flexible print wiring board base material according to claim 1 is characterized in that with the preparation method of two-way stretch Kapton: the said vertical stretch ratio that draws is 1:1.1, and the said horizontal stretch ratio that draws is 1:1.08.
7. a kind of flexible print wiring board base material according to claim 1 is characterized in that with the preparation method of two-way stretch Kapton: the stoste of preparation is brown transparent colloid in the said step (1), and viscosity is 180PaS ~ 220PaS.
8. a flexible print wiring board base material is used the two-way stretch Kapton, it is characterized in that: the Kapton of preparation as stated above, and its thickness is 12.75 microns, thickness deviation is less than ± 0.5mm, apparently is golden yellow; Endwise tensile strength>=200MPa; Transverse tensile strength>=210MPa; Elongation at break 35% ~ 40%; Linear expansivity 40 * 10
-5
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| CN2011102482946A CN102391532B (en) | 2011-08-26 | 2011-08-26 | Biaxially oriented polyimide film for flexible printed circuit board base material and preparation method of biaxially oriented polyimide film |
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| CN102391532B CN102391532B (en) | 2012-11-14 |
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| CN103539957A (en) * | 2013-10-18 | 2014-01-29 | 莱芜中天绝缘材料有限公司 | Treatment method of polyimide film |
| CN103755957A (en) * | 2013-12-30 | 2014-04-30 | 深圳市惠程电气股份有限公司 | High-strength polyimide nano fiber biaxial tension film as well as preparation method and application thereof |
| CN104191633A (en) * | 2014-08-27 | 2014-12-10 | 桂林电器科学研究院有限公司 | Cold processing process and polyimide film production line for manufacturing polyimide film |
| CN104448362A (en) * | 2014-04-23 | 2015-03-25 | 六安市杜尔邦绝缘材料有限公司 | Preparation method of polyimide film |
| CN104448363A (en) * | 2014-04-23 | 2015-03-25 | 六安市杜尔邦绝缘材料有限公司 | Process flow for preparing polyimide film |
| CN105374967A (en) * | 2015-12-18 | 2016-03-02 | 江苏安瑞达新材料有限公司 | Technological method for eliminating rolling stress of microporous membrane of lithium battery |
| CN106009008A (en) * | 2016-04-13 | 2016-10-12 | 安徽鑫柏格电子股份有限公司 | Polyimide film with low dielectric constant and preparation method thereof |
| CN106893121A (en) * | 2015-12-17 | 2017-06-27 | 深圳瑞华泰薄膜科技有限公司 | A kind of Dimensionally-stablepolyimide polyimide film high and preparation method thereof |
| CN107400251A (en) * | 2017-07-27 | 2017-11-28 | 浙江清和新材料科技有限公司 | The preparation method of Kapton used for flexible printed circuit board |
| CN110253904A (en) * | 2019-07-18 | 2019-09-20 | 桂林电器科学研究院有限公司 | A kind of thick polyimide film or super thick film and preparation method thereof |
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| CN110698857A (en) * | 2019-11-30 | 2020-01-17 | 潍坊弘润新材料有限公司 | Biaxially oriented polyimide film for flexible printed circuit board base material and preparation method 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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| CN103539957A (en) * | 2013-10-18 | 2014-01-29 | 莱芜中天绝缘材料有限公司 | Treatment method of polyimide film |
| CN103755957B (en) * | 2013-12-30 | 2016-05-18 | 深圳市惠程电气股份有限公司 | High Strength Polyimide nanofiber biaxial stretching film and its preparation method and application |
| CN103755957A (en) * | 2013-12-30 | 2014-04-30 | 深圳市惠程电气股份有限公司 | High-strength polyimide nano fiber biaxial tension film as well as preparation method and application thereof |
| CN104448362A (en) * | 2014-04-23 | 2015-03-25 | 六安市杜尔邦绝缘材料有限公司 | Preparation method of polyimide film |
| CN104448363A (en) * | 2014-04-23 | 2015-03-25 | 六安市杜尔邦绝缘材料有限公司 | Process flow for preparing polyimide film |
| CN104191633A (en) * | 2014-08-27 | 2014-12-10 | 桂林电器科学研究院有限公司 | Cold processing process and polyimide film production line for manufacturing polyimide film |
| CN106893121A (en) * | 2015-12-17 | 2017-06-27 | 深圳瑞华泰薄膜科技有限公司 | A kind of Dimensionally-stablepolyimide polyimide film high and preparation method thereof |
| CN105374967A (en) * | 2015-12-18 | 2016-03-02 | 江苏安瑞达新材料有限公司 | Technological method for eliminating rolling stress of microporous membrane of lithium battery |
| CN105374967B (en) * | 2015-12-18 | 2017-10-24 | 江苏安瑞达新材料有限公司 | It is a kind of to eliminate the process that lithium battery micro-pore septum winds stress |
| CN106009008A (en) * | 2016-04-13 | 2016-10-12 | 安徽鑫柏格电子股份有限公司 | Polyimide film with low dielectric constant and preparation method thereof |
| CN107400251A (en) * | 2017-07-27 | 2017-11-28 | 浙江清和新材料科技有限公司 | The preparation method of Kapton used for flexible printed circuit board |
| CN110253904A (en) * | 2019-07-18 | 2019-09-20 | 桂林电器科学研究院有限公司 | A kind of thick polyimide film or super thick film and preparation method thereof |
| CN110343275A (en) * | 2019-07-18 | 2019-10-18 | 桂林电器科学研究院有限公司 | A kind of preparation method of polyimides ultrathin membrane |
| CN110698857A (en) * | 2019-11-30 | 2020-01-17 | 潍坊弘润新材料有限公司 | Biaxially oriented polyimide film for flexible printed circuit board base material and preparation method 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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