CN111704735A - Ultralow-thermal-expansion-coefficient high-strength polyimide optical film material and preparation method thereof - Google Patents
Ultralow-thermal-expansion-coefficient high-strength polyimide optical film material and preparation method thereof Download PDFInfo
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- 229920001721 polyimide Polymers 0.000 title claims abstract description 33
- 239000000463 material Substances 0.000 title claims abstract description 32
- 239000012788 optical film Substances 0.000 title claims abstract description 25
- 239000004642 Polyimide Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000003292 glue Substances 0.000 claims abstract description 34
- 229920005575 poly(amic acid) Polymers 0.000 claims abstract description 28
- 239000010408 film Substances 0.000 claims abstract description 26
- 238000004528 spin coating Methods 0.000 claims abstract description 16
- 239000000178 monomer Substances 0.000 claims abstract description 13
- 239000000758 substrate Substances 0.000 claims abstract description 13
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000002834 transmittance Methods 0.000 claims abstract description 8
- 150000004985 diamines Chemical class 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 6
- 125000003118 aryl group Chemical group 0.000 claims abstract description 5
- 150000004984 aromatic diamines Chemical class 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 14
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical group OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 7
- WKDNYTOXBCRNPV-UHFFFAOYSA-N bpda Chemical compound C1=C2C(=O)OC(=O)C2=CC(C=2C=C3C(=O)OC(C3=CC=2)=O)=C1 WKDNYTOXBCRNPV-UHFFFAOYSA-N 0.000 claims description 7
- 239000010453 quartz Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 230000009477 glass transition Effects 0.000 claims description 5
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 4
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 4
- 239000003880 polar aprotic solvent Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 2
- VLDPXPPHXDGHEW-UHFFFAOYSA-N 1-chloro-2-dichlorophosphoryloxybenzene Chemical compound ClC1=CC=CC=C1OP(Cl)(Cl)=O VLDPXPPHXDGHEW-UHFFFAOYSA-N 0.000 claims 2
- XPAQFJJCWGSXGJ-UHFFFAOYSA-N 4-amino-n-(4-aminophenyl)benzamide Chemical group C1=CC(N)=CC=C1NC(=O)C1=CC=C(N)C=C1 XPAQFJJCWGSXGJ-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000035484 reaction time Effects 0.000 claims 1
- 230000003287 optical effect Effects 0.000 abstract description 4
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 238000009987 spinning Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 description 6
- ANSXAPJVJOKRDJ-UHFFFAOYSA-N furo[3,4-f][2]benzofuran-1,3,5,7-tetrone Chemical compound C1=C2C(=O)OC(=O)C2=CC2=C1C(=O)OC2=O ANSXAPJVJOKRDJ-UHFFFAOYSA-N 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- SXGMVGOVILIERA-UHFFFAOYSA-N (2R,3S)-2,3-diaminobutanoic acid Natural products CC(N)C(N)C(O)=O SXGMVGOVILIERA-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- -1 norbornadiene anhydride Chemical class 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- PEEHTFAAVSWFBL-UHFFFAOYSA-N Maleimide Chemical compound O=C1NC(=O)C=C1 PEEHTFAAVSWFBL-UHFFFAOYSA-N 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002981 blocking agent Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 150000003949 imides Chemical group 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- 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
- C08G73/14—Polyamide-imides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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Abstract
The invention discloses a high-strength polyimide optical film material with ultralow thermal expansion coefficient and a preparation method thereof, wherein the polyimide optical film material is prepared by performing polycondensation reaction on an aromatic dianhydride monomer, an aromatic diamine monomer containing amido bond and a diamine monomer not containing amido bond to form a polyamic acid glue solution, coating the polyamic acid glue solution on a film in a spinning way, and performing thermal imidization; the invention also discloses a preparation method of the material, the preparation method is simple, and the prepared polyimide film has the advantages of ultralow thermal expansion coefficient, high mechanical strength, good optical transmittance and good thermal stability; the polyimide film material is obtained by a spin-coating method, can be applied to the fields of optical film diffraction lenses, flexible film solar cells, OLED flexible display substrates and the like, and has wide application prospect.
Description
Technical Field
The invention belongs to the field of materials, and particularly relates to a polyimide optical film material with an ultralow thermal expansion coefficient and high strength and a preparation method thereof.
Background
Polyimide is a high-performance condensation polymer containing imide rings on a main chain, and is widely applied to the fields of aerospace, electronic industry, screen display and the like due to high mechanical strength, high electrical resistance, high chemical corrosion resistance and high thermal stability.
However, the traditional polyimide film material has poor thermal dimensional stability and large dimensional change of the material due to environmental temperature change, which severely limits the application of the material in the photoelectric field. There are several pressing requirements for polyimide films with high dimensional stability, such as replacing traditional inorganic materials as the base material of thin film optical elements in lightweight imaging systems; flexible substrates as new generation display screens; as a flexible substrate for solar cells.
Therefore, a polyimide film material with light weight, high dimensional stability, high strength and high thermal stability is urgently needed, so that the polyimide film material becomes a new generation of basic material in light-weight optical systems, flexible displays and solar cell technologies.
Disclosure of Invention
In order to solve the above problems, an object of the present invention is to provide a polyimide optical film material with high thermal dimensional stability and high strength: the second purpose of the invention is to provide a preparation method of the polyimide optical film material with high thermal dimension stability and high strength, wherein the thermal expansion coefficient of the prepared polyimide film at-150 to 100 ℃ is-2 ppm to 5 ppm/DEG C; the tensile strength is 200-250 MPa; the glass transition temperature is 280-380 ℃; the average transmittance at 500 to 800nm is 70 to 80%.
In order to achieve the above purpose, the invention provides the following technical scheme: a high-strength polyimide optical film material with ultralow thermal expansion coefficient is prepared from aromatic diamine and aromatic dianhydride monomers in a molar ratio of 1: (0.98-1.02) to form polyamic acid glue solution, adding segment end capping agent to control segment molecular weight after reaching certain molecular weight, and obtaining the polyamic acid glue solution through spin coating to form film and thermal imidization.
In the invention, the initial stage of the polycondensation reaction needs to be carried out at a lower temperature, the reaction temperature is selected to be 0-25 ℃, and the polycondensation time is 24-48 hours.
In the invention, the end capping agent is added after the polycondensation reaction is finished to control the viscosity (molecular weight) of the glue solution, so that the mechanical property of the film after film formation can be effectively controlled, and the optical uniformity of the film after subsequent spin coating is facilitated. The end-capping reagent can be isophthalic acid, acetylene, 3- (3-phenylacetylene phenolic group), norbornadiene anhydride, maleimide and allyl norbornadiene.
In the invention, the aromatic dianhydride is one or a mixture of BPDA and PMDA;
the diamine is one or a mixture of more of diamine DABA containing amide bonds and TMDB;
the thermal expansion coefficient of the polyimide optical film material at-150 to 100 ℃ is-2 ppm to 5 ppm/DEG C; the tensile strength is 200-250 MPa; the glass transition temperature is 280-380 ℃; the average transmittance at 500 to 800nm is 70 to 80%.
The invention also aims to provide a preparation method of the polyimide optical film material, which comprises the following steps: under the protection of nitrogen, dispersing diamine monomer containing amido bond in polar aprotic solvent, stirring and dissolving, adding dianhydride monomer in batches, wherein the molar ratio of the diamine monomer to the dianhydride monomer is 1: (0.98-1.02), adding an end-capping reagent to control the molecular weight of the glue solution after the reaction is finished, wherein the solid content of the polyamic acid glue solution is 7% -10%, and stirring for 24-48 hours at 0-25 ℃ to obtain the polyamic acid solution.
Preferably selecting the glue solution, filtering and removing bubbles, and finally spin-coating the polyamic acid glue solution on a quartz substrate with a better surface type to form a film, and performing thermal imidization and substrate removal to obtain the polyimide optical film material with good comprehensive performance
The polar aprotic solvent is a mixed solvent formed by mixing any one or more of N-methylpyrrolidone, N, N-dimethylformamide and N, N-dimethylacetamide in any proportion.
The invention has the following effective effects: the polyimide optical film material with ultralow thermal expansion coefficient and high strength has ultralow thermal expansion coefficient, high mechanical strength, high heat resistance and high transmittance, and the thermal expansion coefficient of-150-100 ℃ is-2 ppm-5 ppm/DEG C; the tensile strength is 200-250 MPa; the glass transition temperature is 280-380 ℃; the average transmittance at 500-800 nm is 70-80%, and the film can be applied to the fields of optical film diffraction lenses, flexible film solar cells, OLED flexible display substrates and the like, and has wide application prospects.
Drawings
In order to make the purpose, technical scheme and beneficial effect of the invention more clear, the invention provides the following drawings:
FIG. 1 is a graph showing the results of the measurement of the change in the thermal expansion dimension of the polyimide film of example 1 using the PMDA/BPDA-TMDB system, which shows that the coefficient of thermal expansion is-0.95 ppm/deg.C at-150 to 100 deg.C.
FIG. 2 is a graph showing five times the results of the tensile strength test of the polyimide film of example 1 using the PMDA/BPDA-TMDB system, and the average tensile strength of the test results is calculated to be 250 MPa.
Detailed Description
Preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings. The test methods in the examples, in which the specific conditions are not specified, are generally carried out under the conventional conditions or under the conditions recommended by the manufacturers.
Example 1
Introducing nitrogen into a 500ml three-neck round-bottom flask equipped with a stirrer, adding 0.050mol of TMDB, dissolving the TMDB in 240g N N-dimethylacetamide, then respectively adding 0.0245mol of PMDA and 0.0245mol of BPDA, keeping the reaction temperature at 0 ℃, continuously stirring for reaction for 30min, reacting for 24-48 h at room temperature, adding an end-capping agent of isophthalic acid after the reaction is finished, continuously stirring for 30min to obtain a polyamic acid glue solution with the solid content of 10.0%, pressurizing and filtering the obtained glue solution, and removing bubbles of the obtained polyamic acid glue solution in vacuum; spin-coating a polyamic acid glue solution wet film with a certain thickness on a quartz substrate by using a spin-coating machine, pre-drying by a heating plate, then baking for 1 hour at 100 ℃, 1 hour at 200 ℃ and 1 hour at 350 ℃ in a vacuum oven by temperature programming, and demoulding to obtain a uniform film with the thickness of 25 mu m after the thermal imidization process is finished. The obtained film was subjected to thermal expansion coefficient and tensile strength tests, and the results are shown in fig. 1 and 2.
Example 2
Introducing nitrogen into a 500ml three-neck round-bottom flask equipped with a stirrer, adding 0.050mol of DABA, dissolving in 240g N-methyl pyrrolidone, then respectively adding 0.025mol of PMDA and 0.025mol of BPDA, keeping the reaction temperature at 0 ℃, continuously stirring for reaction for 30min, reacting at room temperature for 24-48 h, adding an end-capping agent isophthalic acid after the reaction is finished, continuously stirring for 30min to obtain a polyamic acid glue solution with the solid content of 10.0%, pressurizing and filtering the obtained glue solution, and removing bubbles of the obtained polyamic acid glue solution in vacuum; spin-coating a polyamic acid glue solution wet film with a certain thickness on a quartz substrate by using a spin-coating machine, pre-drying by a heating plate, then baking for 1 hour at 100 ℃, 1 hour at 200 ℃ and 1 hour at 350 ℃ in a vacuum oven by temperature programming, and demoulding to obtain a uniform film with the thickness of 20 mu m after the thermal imidization process is finished. The obtained film was subjected to thermal expansion coefficient and tensile strength tests, and the results were similar to those of FIGS. 1 and 2.
Example 3
Introducing nitrogen into a 500ml three-neck round-bottom flask equipped with a stirrer, adding 0.040mol of TMDB, dissolving in 240g N, N-dimethylacetamide, then respectively adding 0.041mol of BPDA, keeping the reaction temperature at 0 ℃, continuously stirring for reaction for 30min, reacting at room temperature for 24-48 h, adding an end-capping agent of isophthalic acid after the reaction is finished, continuously stirring for 30min to obtain a polyamic acid glue solution with the solid content of 8.0%, pressurizing and filtering the obtained glue solution, and removing bubbles of the obtained polyamic acid glue solution in vacuum; spin-coating a polyamic acid glue solution wet film with a certain thickness on a quartz substrate by using a spin-coating machine, pre-drying by a heating plate, then baking for 1 hour at 100 ℃, 1 hour at 200 ℃ and 1 hour at 350 ℃ in a vacuum oven by temperature programming, and demoulding to obtain a uniform film with the thickness of 20 mu m after the thermal imidization process is finished. The obtained film was subjected to thermal expansion coefficient and tensile strength tests, and the results were similar to those of FIGS. 1 and 2.
Example 4
Introducing nitrogen into a 500ml three-neck round-bottom flask equipped with a stirrer, adding 0.020mol TMDB and 0.020mol DABA, dissolving the nitrogen into 240g N-methyl pyrrolidone, then respectively adding 0.0205mol of BPDA and 0.0205mol of PMDA, keeping the reaction temperature at 0 ℃, continuously stirring for reacting for 60min, reacting for 24-48 h at room temperature, adding a blocking agent 3- (3-phenylacetylene phenol group) after the reaction is finished, continuously stirring for 30min to obtain a polyamic acid glue solution with the solid content of 8.0%, pressurizing and filtering the obtained polyamic acid glue solution, and removing bubbles from the obtained polyamic acid glue solution in vacuum; spin-coating a polyamic acid glue solution wet film with a certain thickness on a quartz substrate by using a spin-coating machine, pre-drying by a heating plate, then baking for 1 hour at 100 ℃, 1 hour at 200 ℃ and 1 hour at 350 ℃ in a vacuum oven by temperature programming, and demoulding to obtain a uniform film with the thickness of 15 mu m after the thermal imidization process is finished. The obtained film was subjected to thermal expansion coefficient and tensile strength tests, and the results were similar to those of FIGS. 1 and 2.
Example 5
Introducing nitrogen into a 500ml three-neck round-bottom flask equipped with a stirrer, adding 0.0175mol TMDB and 0.0175mol DABA, dissolving the mixture in 240g N N-dimethylformamide, then respectively adding 0.0357mol BPDA, keeping the reaction temperature at 0 ℃, continuously stirring for reaction for 30min, reacting for 24-48 h at room temperature, adding an end-capping agent of norbornadic anhydride after the reaction is finished, continuously stirring for 30min to obtain a polyamic acid glue solution with the solid content of 7.0%, pressurizing and filtering the obtained glue solution, and removing bubbles of the obtained polyamic acid glue solution in vacuum; spin-coating a polyamic acid glue solution wet film with a certain thickness on a quartz substrate by using a spin-coating machine, pre-drying by a heating plate, then baking for 1 hour at 100 ℃, 1 hour at 200 ℃ and 1 hour at 300 ℃ in a vacuum oven by temperature programming, and demoulding to obtain a uniform film with the thickness of 28 microns after the thermal imidization process is finished. The obtained film was subjected to thermal expansion coefficient and tensile strength tests, and the results were similar to those of FIGS. 1 and 2.
TABLE 1 polyimide optical film Performance test
| Tensile Strength (MPa) | CTE(ppm/℃) | Tg(℃) | Transmittance (%) of 500 to 800nm | |
| Example 1 | 250 | 0.9 | 380 | 80 |
| Example 2 | 245 | -2 | 350 | 77 |
| Example 3 | 200 | 5 | 330 | 72 |
| Example 4 | 220 | 3 | 280 | 73 |
| Example 5 | 210 | 1.5 | 300 | 79 |
The result shows that the thermal expansion coefficient of the polyimide optical film material at-150 to 100 ℃ is-2 ppm to 5 ppm/DEG C; the tensile strength is 200-250 MPa; the glass transition temperature is 280-380 ℃; the average transmittance at 500 to 800nm is 70 to 80%.
Finally, it is noted that the above-mentioned preferred embodiments illustrate rather than limit the invention, and that, although the invention has been described in detail with reference to the above-mentioned preferred embodiments, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the scope of the invention as defined by the appended claims.
Claims (6)
1. An ultralow-thermal-expansion-coefficient high-strength polyimide optical film material is characterized in that: the polyimide optical film material is prepared by mixing aromatic diamine and aromatic dianhydride monomers in a molar ratio of 1: (0.98-1.02) to form polyamic acid glue solution, adding segment end capping agent to control segment molecular weight after reaching certain molecular weight, and obtaining the polyamic acid glue solution through spin coating to form film and thermal imidization.
2. The ultralow cte, high strength polyimide optical film material of claim 1, wherein: the aromatic dianhydride is one or two of 3,3',4,4' -biphenyl tetracarboxylic dianhydride (BPDA) and pyromellitic dianhydride (PMDA); the aromatic diamine is 4,4' -Diaminobenzanilide (DABA) containing amide bonds and diamine 2,2 ' -dimethyl-4, 4' -diaminobiphenyl (TMDB) containing no amide bonds; the end-capping agent is isophthalic acid.
3. The ultra-low coefficient of thermal expansion high strength polyimide optical film material of claim 2, wherein: the thermal expansion coefficient of the polyimide optical film material at-150 to 100 ℃ is-2 ppm to 5 ppm/DEG C; the tensile strength is 200-250 MPa; the glass transition temperature is 280-380 ℃; the average transmittance at 500 to 800nm is 70 to 80%.
4. A preparation method of a polyimide optical film material is characterized by comprising the following steps: under the protection of nitrogen, dispersing diamine monomer containing amido bond in polar aprotic solvent, stirring and dissolving, adding dianhydride monomer in batches, wherein the molar ratio of the diamine monomer to the dianhydride monomer is 1: (0.98-1.02), after the reaction is finished, adding a capping agent to control the molecular weight of the glue solution, controlling the solid content of the polyamic acid glue solution to be 7% -10%, stirring for 24-48 hours at the temperature of 0-25 ℃ to obtain a polyamic acid solution, spin-coating the polyamic acid glue solution on a quartz substrate with a good surface type to form a film, and performing thermal imidization and substrate removal to obtain the polyimide optical film material with good comprehensive performance.
5. The method for producing a polyimide optical film material according to claim 4, characterized in that: the temperature of the polycondensation reaction is 0-25 ℃, and the polycondensation reaction time is 24-48 hours.
6. The method for preparing a polyimide optical film material according to claim 4, wherein the polar aprotic solvent is one or more of N-methylpyrrolidone, N, N-dimethylformamide and N, N-dimethylacetamide mixed in any proportion.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113861481A (en) * | 2021-09-24 | 2021-12-31 | 中国科学院光电技术研究所 | High-transmittance hydrophobic optical polyimide composite film material and preparation method thereof |
| CN114015091A (en) * | 2021-11-12 | 2022-02-08 | 中国科学院长春应用化学研究所 | Polyimide film with low thermal expansion coefficient and preparation method thereof |
| CN114380997A (en) * | 2021-12-16 | 2022-04-22 | 奥克控股集团股份公司 | Preparation method of high-temperature-resistant polyimide film with low thermal expansion coefficient |
| CN114685786A (en) * | 2020-12-25 | 2022-07-01 | 中国科学院化学研究所 | Polyimide film and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106084223A (en) * | 2016-07-01 | 2016-11-09 | 江汉大学 | A kind of method preparing polyimides |
| CN106928707A (en) * | 2015-12-31 | 2017-07-07 | 株式会社东进世美肯 | Polyimide polymer composition, method for producing same, and polyimide film |
| JP2019206705A (en) * | 2014-06-02 | 2019-12-05 | 東洋紡株式会社 | Method for producing polyimide-based film |
-
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2019206705A (en) * | 2014-06-02 | 2019-12-05 | 東洋紡株式会社 | Method for producing polyimide-based film |
| CN106928707A (en) * | 2015-12-31 | 2017-07-07 | 株式会社东进世美肯 | Polyimide polymer composition, method for producing same, and polyimide film |
| CN106084223A (en) * | 2016-07-01 | 2016-11-09 | 江汉大学 | A kind of method preparing polyimides |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114685786A (en) * | 2020-12-25 | 2022-07-01 | 中国科学院化学研究所 | Polyimide film and preparation method and application thereof |
| CN114685786B (en) * | 2020-12-25 | 2023-05-02 | 中国科学院化学研究所 | Polyimide film and preparation method and application thereof |
| CN113861481A (en) * | 2021-09-24 | 2021-12-31 | 中国科学院光电技术研究所 | High-transmittance hydrophobic optical polyimide composite film material and preparation method thereof |
| CN114015091A (en) * | 2021-11-12 | 2022-02-08 | 中国科学院长春应用化学研究所 | Polyimide film with low thermal expansion coefficient and preparation method thereof |
| CN114380997A (en) * | 2021-12-16 | 2022-04-22 | 奥克控股集团股份公司 | Preparation method of high-temperature-resistant polyimide film with low thermal expansion coefficient |
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| CN111704735B (en) | 2023-05-26 |
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