Classifications

• • 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
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B32—LAYERED PRODUCTS
  • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
  • B32B15/00—Layered products comprising a layer of metal
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B32—LAYERED PRODUCTS
  • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
  • B32B27/00—Layered products comprising a layer of synthetic resin
  • B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B32—LAYERED PRODUCTS
  • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
  • B32B27/00—Layered products comprising a layer of synthetic resin
  • B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
  • B32B27/281—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polyimides
• • 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
• • 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
  • C08G73/1042—Copolyimides derived from at least two different tetracarboxylic compounds or two different diamino compounds
• • 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
• • 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

Definitions

• the present invention relates to a polyimide film having a high heat resistance property, a low dielectric property, and a low moisture absorption property, and a method of manufacturing the same.
• Polyimide (PI) is a polymer material that has the highest level of heat resistance, chemical resistance, electrical insulation, chemical resistance, and weather resistance among organic materials based on an imide ring that has excellent chemical stability with a rigid aromatic backbone. to be.
• Such thin circuit boards tend to use a structure in which a circuit including a metal foil is formed on a polyimide film that is easily bent while having excellent heat resistance, low temperature resistance, and insulation characteristics.
• a flexible metal clad laminate is mainly used, and an example includes a flexible copper clad laminate (FCCL) using a thin copper plate as a metal foil.
• FCCL flexible copper clad laminate
• polyimide is also used as a protective film and insulating film for thin circuit boards.
• an insulator having a high impedance capable of maintaining electrical insulation even at high frequencies. Since impedance is inversely proportional to the frequency and dielectric constant (Dk) formed in the insulator, the dielectric constant must be as low as possible in order to maintain insulation even at high frequencies.
• Dk dielectric constant
• the dielectric properties are not excellent enough to maintain sufficient insulation in high-frequency communication.
• polyimide with low dielectric properties is recognized as an important factor in the performance of thin circuit boards.
• the dielectric dissipation factor (Df) refers to the degree of wasted electrical energy of a thin circuit board, and is closely related to the signal transmission delay that determines the communication speed, so it is also possible to keep the dielectric loss rate of polyimide as low as possible. It is recognized as an important factor in the performance of the substrate.
• the polyimide film is suitable as a material for a thin circuit board due to its excellent intrinsic properties, but may be relatively vulnerable to moisture due to polar imide groups, and thus insulation properties may be deteriorated.
• an object of the present invention is to provide a polyimide film having high heat resistance, low dielectric characteristics, and low moisture absorption characteristics, and a method of manufacturing the same.
• the present invention has a practical purpose to provide a specific embodiment thereof.
• One embodiment of the present invention for achieving the above object is benzophenone tetracarboxylic dianhydride (3,3',4,4'-Benzophenonetetracarboxylic dianhydride, BTDA) and biphenyltetracarboxylic dianhydride (3,3',4,4'-Biphenyltetracarboxylic dianhydride, BPDA) containing a dianhydride component and paraphenylene diamine (p-Phenylenediamine, PPD) a first block obtained by the imidization reaction of the diamine component including the; And
• the second obtained by imidization reaction of a dianhydride component including benzophenone tetracarboxylic dianhydride and pyromellitic dianhydride (PMDA) and a diamine component including m-tolidine It provides a polyimide film comprising a block copolymer including;
• the content of m-tolidine is 10 mol% or more and 50 mol% or less, and the content of paraphenylene diamine is 50 mol% or more, based on 100 mol% of the total content of the diamine component of the first block and the second block. It may be less than or equal to mole %.
• the content of benzophenone tetracarboxylicdianhydride is 25 mol% or more and 45 mol% or less, based on 100 mol% of the total content of the dianhydride component of the first block and the second block, and biphenyltetracarboxyl
• the content of rickdian hydride may be 25 mol% or more and 45 mol% or less
• the content of pyromellitic dianhydride may be 15 mol% or more and 40 mol% or less.
• the polyimide film may have a dielectric loss factor (Df) of 0.004 or less, a thermal expansion coefficient (CTE) of 15 ppm/°C or less, and a glass transition temperature (Tg) of 320°C or more.
• Df dielectric loss factor
• CTE thermal expansion coefficient
• Tg glass transition temperature
• Another embodiment of the present invention includes the steps of (a) polymerizing a first dianhydride component and a first diamine component in an organic solvent to prepare a first polyamic acid;
• the first dianhydride component includes benzophenone tetracarboxylic dianhydride and biphenyl tetracarboxylic dianhydride,
• the second dianhydride component includes benzophenone tetracarboxylic dianhydride and pyromellitic dianhydride,
• the first diamine component includes paraphenylene diamine
• the second diamine component provides a method for producing a polyimide film containing m-tolidine.
• the present invention provides a polyimide film having high heat resistance, low dielectric properties, and low moisture absorption through a polyimide film composed of a specific component and a specific composition ratio, and a manufacturing method thereof. It can be usefully applied to various fields, especially electronic components such as flexible metal foil laminates.
• Ranges of numerical values are intended to include the endpoints and all integers and fractions within that range, unless stated otherwise, when a range is referred to herein. It is intended that the scope of the invention is not limited to the specific values recited when defining the range.
• dianhydric acid is intended to include a precursor or derivative thereof, which may not technically be a dianhydride acid, but nevertheless will react with a diamine to form a polyamic acid, and the polyamic acid is again polyamic acid. Can be converted to mid.
• diamine is intended to include precursors or derivatives thereof, which may not technically be diamines, but nevertheless will react with dianhydride to form polyamic acid, which polyamic acid is again polyamic acid. Can be converted to mid.
• the polyimide film according to the present invention is a diamine containing a dianhydride component including benzophenonetetracarboxylicdianhydride (BTDA) and biphenyltetracarboxylic dianhydride (BPDA) and paraphenylene diamine (PPD).
• BTDA benzophenonetetracarboxylicdianhydride
• BPDA biphenyltetracarboxylic dianhydride
• PPD paraphenylene diamine
• the content of m-tolidine is 10 mol% or more and 50 mol% or less, and the content of paraphenylene diamine is 50 mol% or more, based on 100 mol% of the total content of the diamine component of the first block and the second block.
• a first block obtained by imidization reaction of a dianhydride component including biphenyltetracarboxylic dianhydride (BPDA) and a diamine component including paraphenylene diamine (PPD);
• BPDA biphenyltetracarboxylic dianhydride
• PPD paraphenylene diamine
• the content of m-tolidine is 10 mol% or more and 50 mol% or less, and the content of paraphenylene diamine is 50 mol% or more, based on 100 mol% of the total content of the diamine component of the first block and the second block. It may be less than or equal to mole %.
• m-tolidine has a hydrophobic methyl group, which contributes to the low moisture absorption properties of the polyimide film.
• the content of benzophenone tetracarboxylicdianhydride is 25 mol% or more and 45 mol% or less, based on 100 mol% of the total content of the dianhydride component of the first block and the second block, and biphenyltetracarboxyl
• the content of rickdian hydride may be 25 mol% or more and 45 mol% or less
• the content of pyromellitic dianhydride may be 15 mol% or more and 40 mol% or less.
• the content of the benzophenone tetracarboxylic dianhydride is 25 mol% or more and 40 mol% or less
• the content of the biphenyl tetracarboxylic dianhydride is 30 mol% or more and 45 mol% or less
• pyromellitic dian It is preferable that the content of hydride is 20 mol% or more and 40 mol% or less.
• the polyimide chain derived from the biphenyltetracarboxylic dianhydride of the present invention has a structure named as a charge transfer complex (CTC), that is, an electron donor and an electron acceptor. They have regular linear structures that are located close to each other, and intermolecular interactions are strengthened.
• CTC charge transfer complex
• benzophenonetetracarboxylicdianhydride which has a carbonyl group, also contributes to the expression of CTC like biphenyltetracarboxylicdianhydride.
• this structure Since this structure has an effect of preventing hydrogen bonding with moisture, it has an effect on lowering the moisture absorption rate, thereby maximizing the effect of lowering the hygroscopicity of the polyimide film.
• the dianhydride component may additionally include pyromellitic dianhydride.
• Pyromellitic dianhydride is a dianhydride component having a relatively rigid structure and is preferable in that it can impart appropriate elasticity to the polyimide film.
• the content ratio of dianhydride is particularly important. For example, as the content ratio of biphenyltetracarboxylic dianhydride decreases, it becomes difficult to expect a low moisture absorption rate due to the CTC structure.
• biphenyltetracarboxylic dianhydride and benzophenone tetracarboxylicdianhydride contain two benzene rings corresponding to the aromatic moiety
• pyromellitic dianhydride contains benzene rings corresponding to the aromatic moiety. I include one.
• the increase in the content of pyromellitic dianhydride in the dianhydride component increases the imide group in the molecule based on the same molecular weight, which is an image derived from the pyromellitic dianhydride in the polyimide polymer chain. It can be understood that the ratio of the radical increases relative to the imide group derived from biphenyltetracarboxylic dianhydride and benzophenonetetracarboxylicdianhydride.
• the increase in the content of pyromellitic dianhydride can be seen as a relative increase in the imide group even for the entire polyimide film, which makes it difficult to expect a low moisture absorption rate.
• the component of a relatively rigid structure decreases, so that the elasticity of the polyimide film may be lowered to a desired level or less.
• the polyimide film may have a dielectric loss factor (Df) of 0.004 or less, a thermal expansion coefficient (CTE) of 15 ppm/°C or less, and a glass transition temperature (Tg) of 320°C or more.
• Df dielectric loss factor
• CTE thermal expansion coefficient
• Tg glass transition temperature
• a polyimide film that satisfies all of the dielectric loss rate (Df), glass transition temperature, and moisture absorption rate, it can be used as an insulating film for a flexible metal clad laminate, and the manufactured flexible metal clad laminate transmits a signal at a high frequency of 10 GHz or higher. Even if it is used as a transmitting electrical signal transmission circuit, its insulation stability can be ensured, and signal transmission delay can also be minimized.
• the polyimide film having all of the above conditions is a novel polyimide film that has not been known so far, and the dielectric loss factor (Df) will be described in detail below.
• Dielectric loss rate means the force dissipated by the dielectric (or insulator) when the friction of the molecules interferes with the molecular motion caused by the alternating electric field.
• the value of the dielectric loss rate is commonly used as an index indicating the ease of dissipation (dielectric loss), and the higher the dielectric loss rate, the easier it is to dissipate the charge. Conversely, the lower the dielectric loss rate, the more difficult it is to dissipate the charge. have. That is, since the dielectric loss rate is a measure of the power loss, the lower the dielectric loss rate, the faster the communication speed can be maintained while the signal transmission delay due to the power loss is alleviated.
• the polyimide film which is an insulating film
• the polyimide film according to the present invention may have a dielectric loss rate of 0.004 or less under a very high frequency of 10 GHz.
• the polymerization method is not limited to the above examples, and of course, any known method may be used to prepare the first to third polyamic acids.
• the first dianhydride component includes benzophenone tetracarboxylic dianhydride and biphenyl tetracarboxylic dianhydride,
• the second dianhydride component includes benzophenonetetracarboxylicdianhydride and pyromellitic dianhydride
• the first diamine component includes paraphenylene diamine
• the second diamine component includes m-tolidine.
• the content of m-tolidine is 10 mol% or more and 50 mol% or less, and the content of paraphenylene diamine is 50 mol% It may be more than 90 mol% or less.
• the content of benzophenonetetracarboxylicdianhydride is 25 mol% or more and 45 mol% or less, based on 100 mol% of the total content of the dianhydride component of the first polyamic acid and the second polyamic acid, and biphenyltetra
• the content of carboxylic dianhydride may be 25 mol% or more and 45 mol% or less
• the content of pyromellitic dianhydride (PMDA) may be 15 mol% or more and 40 mol% or less.
• the polymerization method of the polyamic acid as described above can be defined as a random polymerization method, and the polyimide film prepared from the polyamic acid of the present invention prepared by the above process has a dielectric loss factor (Df) and It can be preferably applied in terms of maximizing the effect of the present invention to lower the moisture absorption rate.
• Df dielectric loss factor
• the polymerization method of the polyamic acid that can be particularly preferably used in the present invention may be a block polymerization method.
• the solvent for synthesizing the polyamic acid is not particularly limited, and any solvent may be used as long as it dissolves the polyamic acid, but it is preferably an amide solvent.
• the solvent may be an organic polar solvent, specifically an aprotic polar solvent, for example, N,N-dimethylformamide (DMF), N,N- It may be one or more selected from the group consisting of dimethylacetamide, N-methyl-pyrrolidone (NMP), gamma butyrolactone (GBL), and Diglyme, but is not limited thereto, and alone or as needed. It can be used in combination of two or more.
• DMF N,N-dimethylformamide
• NMP N-methyl-pyrrolidone
• GBL gamma butyrolactone
• Diglyme but is not limited thereto, and alone or as needed. It can be used in combination of two or more.
• N,N-dimethylformamide and N,N-dimethylacetamide may be particularly preferably used as the solvent.
• a filler may be added for the purpose of improving various properties of the film such as sliding properties, thermal conductivity, corona resistance, and loop hardness.
• the filler to be added is not particularly limited, but preferred examples include silica, titanium oxide, alumina, silicon nitride, boron nitride, calcium hydrogen phosphate, calcium phosphate, mica, and the like.
• the particle diameter of the filler is not particularly limited, and may be determined according to the film properties to be modified and the type of filler to be added. In general, the average particle diameter is 0.05 to 100 ⁇ m, preferably 0.1 to 75 ⁇ m, more preferably 0.1 to 50 ⁇ m, and particularly preferably 0.1 to 25 ⁇ m.
• the particle diameter is less than this range, the modification effect is difficult to appear, and if it exceeds this range, the surface properties may be greatly impaired, or the mechanical properties may be greatly reduced.
• the amount of the filler added is not particularly limited, and may be determined according to the film properties to be modified, the filler particle size, or the like. In general, the amount of the filler added is 0.01 to 100 parts by weight, preferably 0.01 to 90 parts by weight, more preferably 0.02 to 80 parts by weight, based on 100 parts by weight of the polyimide.
• the amount of the filler added is less than this range, the effect of modifying by the filler is difficult to appear, and if it exceeds this range, there is a possibility that the mechanical properties of the film will be greatly impaired.
• the method of adding the filler is not particularly limited, and any known method may be used.
• the polyimide film may be manufactured by thermal imidization and chemical imidization.
• it may be produced by a composite imidization method in which a thermal imidation method and a chemical imidization method are combined.
• the thermal imidation method is a method of inducing an imidation reaction with a heat source such as hot air or an infrared dryer, excluding a chemical catalyst.
• the gel film may be heat-treated at a variable temperature in the range of 100 to 600° C. to imidize the amic acid group present in the gel film, and in detail, 200 to 500° C., more specifically, The amic acid group present in the gel film may be imidized by heat treatment at 300 to 500°C.
• the polyamic acid composition may be dried at a variable temperature in the range of 50 °C to 200 °C. It can be, and this can also be included in the category of the thermal imidization method.
• a polyimide film may be prepared by using a dehydrating agent and an imidizing agent according to a method known in the art.
• the complex imidization method after adding a dehydrating agent and an imidizing agent to the polyamic acid solution, heating at 80 to 200°C, preferably 100 to 180°C, partially curing and drying, at 200 to 400°C for 5 to 400 seconds By heating, a polyimide film can be produced.
• the polyimide film of the present invention manufactured according to the above manufacturing method has a dielectric loss factor (Df) of 0.004 or less, a thermal expansion coefficient (CTE) of 15 ppm/°C or less, and a glass transition temperature (Tg) of 320°C or more. I can.
• the present invention provides a multilayer film comprising the above-described polyimide film and a thermoplastic resin layer, and a flexible metal foil laminate comprising the above-described polyimide film and an electrically conductive metal foil.
• thermoplastic resin layer for example, a thermoplastic polyimide resin layer or the like may be applied.
• the metal foil to be used is not particularly limited, but when the flexible metal foil laminate of the present invention is used for electronic devices or electric devices, for example, copper or copper alloy, stainless steel or alloy thereof, nickel or nickel alloy (alloy 42 Also included), it may be a metal foil containing aluminum or an aluminum alloy.
• a general flexible metal foil laminate many copper foils such as rolled copper foil and electrolytic copper foil are used, and can be preferably used also in the present invention.
• a rust prevention layer, a heat-resistant layer, or an adhesive layer may be applied to the surface of these metal foils.
• the thickness of the metal foil is not particularly limited, and may be any thickness capable of exhibiting a sufficient function according to the application.
• a metal foil is laminated on one side of the polyimide film, or an adhesive layer containing a thermoplastic polyimide is added to one side of the polyimide film, and the metal foil is attached to the adhesive layer. It may be a laminated structure.
• the present invention also provides an electronic component including the flexible metal foil laminate as an electrical signal transmission circuit.
• the electrical signal transmission circuit may be an electronic component that transmits a signal at a high frequency of at least 2 GHz, in detail, a high frequency of at least 5 GHz, and more particularly, a high frequency of at least 10 GHz.
• the electronic component may be, for example, a communication circuit for a portable terminal, a communication circuit for a computer, or a communication circuit for aerospace, but is not limited thereto.
• NMP NMP was introduced while nitrogen was injected, and the temperature of the reactor was set to 30°C. Ride and pyromellitic dianhydride are added to confirm that they are completely dissolved. After the temperature was raised to 40° C. in a nitrogen atmosphere and stirring was continued for 120 minutes while heating, a second polyamic acid having a viscosity of 200,000 cP at 23° C. was prepared.
• the first polyamic acid and the second polyamic acid were heated to 40° C. in a nitrogen atmosphere, and stirred for 120 minutes while heating, and then the final viscosity at 23° C. was 200,000 cP, and the diamine component and dianhydride acid A third polyamic acid containing components as shown in Table 1 was prepared.
• Air bubbles were removed by rotating the third polyamic acid prepared above at a high speed of 1,500 rpm or more. Thereafter, the defoamed polyimide precursor composition was applied to the glass substrate using a spin coater. Thereafter, a gel film was prepared by drying in a nitrogen atmosphere and at a temperature of 120° C. for 30 minutes, and the gel film was heated to 450° C. at a rate of 2° C./min, heat-treated at 450° C. for 60 minutes, and then until 30° C. It cooled at a rate of 2° C./min to obtain a polyimide film.
• the polyimide film was peeled off from the glass substrate by dipping in distilled water.
• the thickness of the prepared polyimide film was 15 ⁇ m.
• the thickness of the prepared polyimide film was measured using an Anritsu's Electric Film thickness tester.
• Example 1 a polyimide film was prepared in the same manner as in Example 1, except that the components and their contents were respectively changed as shown in Table 1 below.
• Example 1 Dianhydride component (mol%) Diamine component (mol%) Polyamic acid polymerization method BPDA (mol%) BTDA (mol%) PMDA (mol%) m-Tolidine (mol%) PPD (mol%)
• Example 1 40 30 30 20 80 Block polymerization Example 2 35 32 33 30 70 Block polymerization Example 3 40 40 20 20 80 Block polymerization Example 4 44 28 28 12 88 Block polymerization Example 5 30 32 38 40 60 Block polymerization Example 6 35 20 45 48 52 Block polymerization Comparative Example 1 40 17 43 40 60 Block polymerization Comparative Example 2 30 14 56 40 60 Block polymerization Comparative Example 3 35 17 48 30 70 Block polymerization Comparative Example 4 40 20 40 20 80 Block polymerization
• the dielectric loss factor (Df) was measured by leaving the flexible metal foil laminate for 72 hours using an ohmmeter Agilent 4294A.
• CTE coefficient of thermal expansion
• a Q400 model of a thermomechanical analyzer from TA was used, and a polyimide film was cut into a width of 4 mm and a length of 20 mm, and a tension of 0.05 N was applied in a nitrogen atmosphere, while 10 °C/min.
• the slope of the 100°C to 200°C section was measured while cooling at a rate of 10°C/min.
• the glass transition temperature (T g ) was obtained by using DMA to determine the loss modulus and storage modulus of each film, and the inflection point was measured as a glass transition degree in the tangent graph.
• Example 1 0.0036 9.0 358
• Example 2 0.0036 8.5 350
• Example 3 0.0033 12.0 340
• Example 4 0.0035 8.5 348
• Example 5 0.0036 8.1 340
• Example 6 0.0034 7.4 325 Comparative Example 1 0.0041 0.3 326 Comparative Example 2 0.0047 0.3 360 Comparative Example 3 0.0040 3.4 368 Comparative Example 4 0.0043 8.4 350
• the polyimide film prepared according to the embodiment of the present invention not only exhibits a remarkably low dielectric loss rate, such as 0.004 or less, but also has a desired level of thermal expansion coefficient and glass transition temperature.
• the examples show that it is difficult to be used for electronic components in which signals are transmitted at high frequency in giga units in more than one aspect of dielectric loss ratio, coefficient of thermal expansion, and glass transition temperature compared to the polyimide films of Comparative Examples 1 to 4 having different components. Can be expected.
• the present invention provides a polyimide film having high heat resistance, low dielectric properties, and low moisture absorption through a polyimide film composed of a specific component and a specific composition ratio, and a manufacturing method thereof, thereby providing a polyimide film having such characteristics It can be usefully applied to electronic components such as laminates.

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• 2019
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