A method for carrying out a process involving the heating and melting of a heat-resistant release sheet and a resin

Abstract

To provide a heat-resistant release sheet which, when providing a resin or an object including a resin in a process involving heating and melting, is arranged between the resin or the object and a member contacting the resin or the object in the process and prevents direct contact between the resin or the object and the member, which is suitable for preventing occurrence of a problem in the step caused by a cutting sheet of a heat-resistant resin while including the cutting sheet.SOLUTION: A heat-resistant release sheet 1 includes a cutting sheet of polytetrafluoroethylene (PTFE) or modified PTFE. A percentage content of a tetrafluoroethylene (PTFE) unit in the modified PTFE is 99 mass% or more. In each of two directions orthogonal to each other that are in-plane directions of the heat-resistant release sheet, a dimensional shrinkage rate generated by heating at 175°C for 30 minutes exceeds 0%.SELECTED DRAWING: Figure 3

Description

[Technical Field]

[0001] The present invention relates to a heat-resistant release sheet and a method for carrying out a process involving heat melting of a resin using the same. [Background technology]

[0002] Fluorine resins are known as heat-resistant resins. Patent Document 1 discloses a cutting sheet made of polytetrafluoroethylene (hereinafter referred to as "PTFE"), a type of fluororesin. PTFE sheets, which are heat-resistant resin sheets, are expected to be used under high temperatures. [Prior art documents] [Patent documents]

[0003] [Patent Document 1] Japanese Patent Application Laid-Open No. 2001-341138 Summary of the Invention [Problem to be solved by the invention]

[0004] Melt molding of resins using a mold or heat-and-pressure treatment of resin-containing objects using a heat-and-pressure device involves processes involving the heating and melting of resins. In these processes, a heat-resistant release sheet can be placed between the resin or resin-containing object and a component that comes into contact with the resin or object to prevent direct contact between the resin or object and the component. Alternatively, a heat-resistant resin sheet, such as a cut PTFE sheet, can be used as the heat-resistant release sheet. However, the inventors' investigations have revealed that the use of a cut sheet can result in streaky defects on the surface of the molded product obtained by melt molding or a decrease in the uniformity of the heat-and-pressure treatment. In addition to cut sheets, cast PTFE sheets are also available, which are produced by drying and baking a coating of a PTFE dispersion. However, these cast sheets do not suffer from the above-mentioned problems.

[0005] The object of the present invention is to provide a heat-resistant release sheet that, when a resin or an object containing a resin is subjected to a process involving heating and melting the resin, is placed between the resin or object and a member that comes into contact with the resin or object in the process, thereby preventing direct contact between the resin or object and the member, and which, while including a cutting sheet of heat-resistant resin, is suitable for preventing problems in the process caused by the cutting sheet, such as the occurrence of the above-mentioned defects and a decrease in homogeneity. [Means for solving the problem]

[0006] The present invention provides A heat-resistant release sheet that is disposed between a resin or an object containing the resin and a member that comes into contact with the resin or the object in a process involving heat melting of the resin, to prevent direct contact between the resin or the object and the member, when the resin or the object is subjected to the process involving heat melting of the resin, It includes a cutting sheet of polytetrafluoroethylene (PTFE) or modified PTFE, The content of tetrafluoroethylene (TFE) units in the modified PTFE is 99% by mass or more, A heat-resistant release sheet having a dimensional shrinkage rate of more than 0% when heated at 175°C for 30 minutes in each of two mutually perpendicular in-plane directions of the heat-resistant release sheet. to provide.

[0007] From another aspect, the present invention provides a method for manufacturing a semiconductor device comprising: A method for carrying out a process involving heating and melting a resin, a heat-resistant release sheet is placed between the resin or an object containing the resin to be subjected to the process and a member that comes into contact with the resin or the object in the process, and the process is carried out in a state where the heat-resistant release sheet prevents direct contact between the resin or the object and the member, The heat-resistant release sheet is the heat-resistant release sheet of the present invention. to provide. [Effects of the Invention]

[0008] The inventors' investigations have revealed that the above-mentioned problems that can occur when using cut sheets are due to the formation of streaky wrinkles in the cut sheets that extend in a specific direction, typically the MD, caused by heating during resin melting, and that these wrinkles are presumably due to the manufacturing process specific to cut sheets. In the manufacture of cut sheets, raw material powder is preformed into a cylindrical shape or the like, during which strong pressure is applied in one direction. This direction corresponds to the specific direction in which wrinkles will occur after the cut sheet is formed. It is believed that compressive strain due to the pressure applied during preforming remains in the cut sheet and is released by heating, resulting in the formation of streaky wrinkles. On the other hand, the heat-resistant release sheet of the present invention exhibits a dimensional shrinkage rate of more than 0% in each of two mutually perpendicular in-plane directions of the sheet when heated at 175°C for 30 minutes (corresponding to typical heating for melting a resin). This means that the residual compressive strain is suppressed in the heat-resistant release sheet of the present invention. Therefore, the heat-resistant release sheet of the present invention can prevent problems in the above steps caused by the cutting sheet, such as the occurrence of the above defects and deterioration of uniformity. [Brief explanation of the drawings]

[0009] [Figure 1] FIG. 1 is a cross-sectional view schematically illustrating an example of the heat-resistant release sheet of the present invention. [Figure 2] FIG. 2 is a schematic diagram illustrating an example of melt molding of a resin using the heat-resistant release sheet of the present invention. [Figure 3] FIG. 3 is a schematic diagram illustrating an example of a heat and pressure treatment using the heat-resistant release sheet of the present invention. DETAILED DESCRIPTION OF THE INVENTION

[0010] DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described below with reference to the accompanying drawings, but is not limited to the following embodiments.

[0011] [Heat-resistant release sheet] The heat-resistant release sheet of this embodiment is shown in FIG. 1. The heat-resistant release sheet 1 in FIG. 1 is composed of a cut sheet 2 made of PTFE. The heat-resistant release sheet 1 in FIG. 1 has a single-layer structure of the cut sheet 2. The heat-resistant release sheet 1 has high heat resistance and flexibility due to the PTFE contained in the cut sheet 2. The fact that the sheet is a cut sheet can be determined by the presence of linear scratches (known to those skilled in the art as cut scratches) specific to cut sheets when the surface of the sheet is observed under magnification. A microscope such as an optical microscope or a surface texture evaluation device can be used for magnification observation of the surface. Cut scratches occur when resin shavings accumulated on the cutting blade during cutting work cause linear scratches on the sheet surface. Cut scratches typically extend in the MD direction of the cut sheet 2. The MD direction of the strip-shaped cut sheet 2 is typically the longitudinal direction of the sheet.

[0012] In the heat-resistant release sheet 1, the dimensional shrinkage rate (hereinafter referred to as "dimensional shrinkage rate") caused by heating at 175°C for 30 minutes exceeds 0% in each of two mutually perpendicular in-plane directions of the sheet 1. These two directions are typically the MD and TD directions of the cut sheet 2. The TD direction of the strip-shaped cut sheet 2 is usually the width direction of the sheet. The dimensional shrinkage rate is calculated by the formula (X0-X1) / X0×100(%), where X0 is the dimension before heating and X1 is the dimension after heating, measured by leaving the heat-resistant release sheet 1 stationary under heating conditions of 175°C for 30 minutes. The dimensional shrinkage rate in each of the two directions may be 0.5% or more, 1.0% or more, 1.5% or more, 1.7% or more, 1.9% or more, 2.0% or more, 3.0% or more, 4.0% or more, or even 5.0% or more. The upper limit of the dimensional shrinkage rate in each of the two directions may be, for example, 10% or less, and may be 8.0% or less, 7.0% or less, 6.0% or less, 5.0% or less, 4.0% or less, 3.0% or less, 2.5% or less, 2.0% or less, 1.9% or less, or even 1.7% or less. The dimensional shrinkage rates in the two directions may be different from each other. The dimensional shrinkage rates in each direction may independently fall within one range selected from the multiple preferred ranges described above. Furthermore, the difference between the dimensional shrinkage rates in each of the two directions may be less than 5.0%, 4.5% or less, 4.0% or less, 3.5% or less, 3.1% or less, 3.0% or less, 2.5% or less, 2.0% or less, 1.5% or less, 1.0% or less, 0.7% or less, 0.5% or less, or even 0.3% or less. Note that the dimensional shrinkage rate in the TD direction of conventional cutting sheets is 0% or less. In other words, in a conventional cut sheet, the residual compressive strain is released by heating and the sheet expands in the TD direction. On the other hand, in the heat-resistant release sheet 1, the dimensional shrinkage rate in the TD direction may be larger than the dimensional shrinkage rate in the MD direction.

[0013] The heat-resistant release sheet 1 in FIG. 1 includes a cut PTFE sheet 2. However, the heat-resistant release sheet 1 may also include a cut PTFE sheet 2. The modified PTFE cut sheet 2 has excellent heat resistance and flexibility like the cut PTFE sheet 2, and can be produced by the same manufacturing method as the cut PTFE sheet 2. Modified PTFE is a copolymer of TFE and a modified comonomer. To be classified as modified PTFE, the content of tetrafluoroethylene (TFE) units in the copolymer must be 99% by mass or more. The modified PTFE is, for example, a copolymer of TFE and at least one modified comonomer selected from ethylene, perfluoroalkyl vinyl ether, and hexafluoropropylene.

[0014] The cutting sheet 2 is preferably a sintered sheet containing PTFE or modified PTFE that has been sintered. In this specification, sintering means heating the PTFE or modified PTFE obtained by polymerization to a temperature above its melting point (327°C for PTFE), for example, 340 to 380°C.

[0015] The thickness of the heat-resistant release sheet 1 is, for example, 10 μm or more, and may be 20 μm or more, 25 μm or more, 30 μm or more, 40 μm or more, or even 50 μm or more. The upper limit of the thickness is, for example, 500 μm or less, 200 μm or less, or even 100 μm or less.

[0016] The linear thermal expansion coefficient α of the heat-resistant release sheet 1 in the temperature range of 25°C to 175°C in each of the above two directions is 150 x 10 -6 / ℃ or less, 125 × 10 -6 / ℃ or less, 120×10 -6 / ℃ or less, 110×10 -6 / ℃ or less, 100×10 -6 / ℃ or less, 90×10 -6 / ℃ or less, 50×10 -6 / ℃ or less, 30×10 -6 / ℃ or below, even 0×10 -6 / °C or less. The linear thermal expansion coefficient α in the MD direction may be 125×10 -6 / ℃ or less, 120×10 -6 / ℃ or less, 110×10 -6 / ℃ or less, 100×10 -6 / ℃ or less, and even 90×10 -6 / ℃ or less, 0×10 -6 / ℃ or more, 25×10 -6 / ℃ or more, even 50×10 -6 / °C or more. The linear thermal expansion coefficient α in the TD direction may be 125×10 -6 / ℃ or less, 120×10 -6 / ℃ or less, 110×10 -6 / ℃ or less, 100×10 -6 / ℃ or less, 90×10 -6 / ℃ or less, 50×10 -6 / ℃ or less, 30×10 -6 / ℃ or below, even 0×10 -6 / ℃ or less, -400 × 10 -6 / ℃ or more, -300×10 -6 / ℃ or higher, even -200×10 -6 / °C or more. The coefficient of linear thermal expansion α in the TD direction may be a negative value. The coefficient of linear thermal expansion α of the heat-resistant release sheet 1 can be determined by thermomechanical analysis (TMA). TMA may be performed under the following conditions. The average value of values ​​obtained by measuring at least five test pieces can be used as the coefficient of linear thermal expansion α. Measurement temperature range: 25℃-175℃ Mode: Tension mode Test piece: width 4mm x length 20mm Tensile direction: length direction of test piece Tensile load: 2gf Heating rate: 5°C / min Ambient atmosphere of test piece during measurement: "Ambient atmosphere of test piece" as defined in Japan Industrial Standards (formerly Japan Industrial Standards; JIS) K7197:1991 "Test method for linear expansion coefficient by thermomechanical analysis of plastics"

[0017] The heat-resistant release sheet 1 may have a tensile strength of 30 MPa or more and a maximum tensile elongation of 250% or more in each of the two directions. The tensile strength may be 35 MPa or more, 40 MPa or more, 45 MPa or more, 50 MPa or more, or even 55 MPa or more. The upper limit of the tensile strength is, for example, 100 MPa or less. The maximum tensile elongation may be 275% or more, 300% or more, 325% or more, 350% or more, 400% or more, or even 450% or more. The upper limit of the maximum tensile elongation is, for example, 600% or less. The tensile strength and maximum tensile elongation may be any combination of the above-mentioned ranges. A heat-resistant release sheet 1 having a tensile strength and maximum tensile elongation within the above ranges allows the sheet 1 to be more reliably and stably supplied by conveyance, for example, in a process involving heat melting of a resin.

[0018] The tensile strength and maximum tensile elongation of the heat-resistant release sheet 1 can be determined by a tensile test using a tensile tester. The shape of the test piece is, for example, a dumbbell-shaped No. 3 as specified in JIS K6251:1993. When using the above test piece, the measurement conditions are, for example, a gauge length of 20 mm, a chuck distance of 35 mm, and a tensile speed of 200 mm / min. The maximum tensile elongation can be calculated from the gauge length before the test and the gauge length at break. The measurement temperature is, for example, 25±10°C.

[0019] The heat-resistant release sheet 1 may have other layers disposed on at least one of its main surfaces. However, if good thermal conductivity is required for the heat-resistant release sheet 1, it is preferable that no other layers be disposed on the main surface. In other words, the heat-resistant release sheet 1 may be a single layer.

[0020] At least one of the main surfaces, preferably both main surfaces, of the heat-resistant release sheet 1 may be untreated. An example of the surface treatment is an adhesion-improving treatment that improves the adhesiveness (adhesion to other articles) of the main surface of the PTFE sheet or modified PTFE sheet. Examples of the adhesion-improving treatment are plasma treatment, sputtering treatment, and sodium treatment, and particularly plasma treatment.

[0021] The heat-resistant release sheet 1 is preferably a non-porous sheet. The heat-resistant release sheet 1 may be a sheet that does not have holes that connect both main surfaces at least in the use area. The heat-resistant release sheet 1 may be an impermeable sheet that does not allow fluids such as water to pass through in the thickness direction, based on the high liquid repellency (water repellency and oil repellency) of PTFE or modified PTFE. Furthermore, the heat-resistant release sheet 1 may be an insulating sheet (non-conductive sheet) based on the high insulating property of PTFE or modified PTFE. The insulating property may be, for example, 1×10 14 It is expressed by a surface resistivity of Ω / □ or more. Surface resistivity is 1×10 15 Ω / □ or more, 1×10 16 Ω / □ or more, even 1×10 17 The heat-resistant release sheet 1 may have a surface resistivity of Ω / □ or more. The heat-resistant release sheet 1 may contain a conductive material such as carbon black, a conductive polymer, or a conductive metal oxide. In this case, the heat-resistant release sheet 1 may have a function based on the conductive material, such as an antistatic function. The surface resistivity of the heat-resistant release sheet 1 containing the conductive material may be, for example, 1×10 12 Ω / □ or less, 1×10 8 Ω / □ or less, 1×10 4 It may be Ω / □ or less.

[0022] The shape of the heat-resistant release sheet 1 is, for example, a polygon including a square and a rectangle, a circle, an ellipse, or a strip. The corners of the polygon may be rounded. However, the shape of the heat-resistant release sheet 1 is not limited to the above examples. The polygonal, circular, and elliptical heat-resistant release sheets 1 can be distributed as sheets, while the strip-shaped heat-resistant release sheet 1 can be distributed as a roll wound around a core. The width of the strip-shaped heat-resistant release sheet 1 and the width of the roll formed by winding the strip-shaped heat-resistant release sheet 1 can be freely set.

[0023] [Method of manufacturing heat-resistant release sheet] The following describes an example of a method for producing the heat-resistant release sheet 1. However, the method for producing the heat-resistant release sheet 1 is not limited to the example shown below.

[0024] First, PTFE powder (molding powder) is introduced into a mold, and a predetermined pressure is applied to the powder in the mold for a predetermined time to form a preform. Preformation can be performed at room temperature. The shape of the mold's internal space is preferably cylindrical to enable cutting using a cutting lathe, as described below. In this case, the predetermined pressure is usually applied in the height direction of the cylinder. This also results in a cylindrical preform and PTFE block. When the PTFE block is cylindrical, a cutting lathe can be used to continuously cut the surface while rotating the block, allowing for efficient formation of the heat-resistant release sheet 1. Next, the resulting preform is removed from the mold and baked for a predetermined time at a temperature above the melting point of PTFE (327°C) to obtain a PTFE block. The resulting PTFE block is then cut to a predetermined thickness to obtain a cut PTFE sheet. The resulting PTFE sheet is then stretched in the width direction (TD) to obtain a cut PTFE sheet 2, which is a uniaxially stretched sheet in the width direction. Stretching releases the compressive strain in the TD direction. The obtained cut sheet 2 may be used as the heat-resistant release sheet 1 as is, or may be used after undergoing a predetermined treatment or lamination of other layers. A tenter stretching device can be used for stretching. The stretching ratio is, for example, 1.05 to 1.2 times, or may be 1.1 to 1.5 times. When the stretching ratio is within the above range, a cut sheet 2 without holes connecting both main surfaces can be more reliably obtained, and the occurrence of pinholes due to stretching can be suppressed. The stretching temperature is, for example, 150 to 330°C, or may be 200 to 300°C. Note that, according to the above production method, it is relatively easy to control the thickness of the heat-resistant release sheet 1 to be formed, and a strip-shaped heat-resistant release sheet 1 can also be formed. Furthermore, by using modified PTFE powder instead of PTFE powder, a cut sheet 2 of modified PTFE can be formed by the above method.

[0025] [Use of heat-resistant release sheet] The heat-resistant release sheet 1 can be used in processes involving heat melting of resin. Examples of such processes include melt molding of resin using a mold and heat and pressure treatment of an object containing resin using a heat and pressure device. However, processes involving heat melting of resin are not limited to the above examples, as long as a member that comes into contact with the resin or an object containing resin is used in the process.

[0026] An example of melt molding of resin using a mold is shown in FIG. 2. In the example of FIG. 2, heat-resistant release sheet 1 is placed between mold (upper mold in FIG. 2) 12 and resin 13 during melt molding of resin 13, and is used as a sheet to prevent direct contact between the two. Mold 12 is a member that comes into contact with the resin during melt molding. Melt molding in the example of FIG. 2 can be performed by supplying resin 13 between mold (lower mold) 11 and mold 12 and joining the pair of molds 11, 12 together. In this case, heat-resistant release sheet 1 may be adsorbed to the inner surface of mold 12. The supplied resin 13 may be a solid, such as pellets, or a molten resin. The molten resin is usually supplied after the molds 11, 12 have been joined together. However, the mode of melt molding of resin using a heat-resistant release sheet is not limited to the above example.

[0027] The heat-resistant release sheet 1 may be fed and placed between the mold 11 and the mold 12 by conveying. The heat-resistant release sheet 1 fed and placed by conveying may be in a strip shape. In other words, the strip-shaped heat-resistant release sheet 1 may be fed between the molds by conveying, and a step involving heat melting of the resin may be carried out.

[0028] FIG. 3 shows an example of a heat-pressure treatment using a heat-pressure device. In the example of FIG. 3, a heat-resistant release sheet 1 is placed between a heat-pressure surface 34 of a heat-pressure device 31 and a resin-containing object 35 during the heat-pressure treatment of the object 35 by the heat-pressure device 31, and is used as a sheet to prevent direct contact between the two. The heat-pressure device 31 in FIG. 3 includes a stage 32 and a heat-pressure head 33 having a heat-pressure surface 34. The heat-pressure head 33 is a member that comes into contact with the object 35 during the heat-pressure treatment. The heat-resistant release sheet 1 is placed between the heat-pressure head 33 and the object 35. The heat-pressure treatment in the example of FIG. 3 can be performed by placing the object 35 on the stage 32 and bringing the heat-pressure head 33 and the stage 32 closer together (typically by lowering the heat-pressure head 33). The heat-pressure treatment is, for example, thermocompression bonding or heat pressing of the object 35.

[0029] The heat-resistant release sheet 1 may be supplied and placed between the heat pressing surface 34 and the object 35 by conveying. The heat-resistant release sheet 1 supplied and placed by conveying may be in a strip shape. In other words, the strip-shaped heat-resistant release sheet 1 may be supplied to the heat pressing device by conveying, and a process involving heat melting of the resin may be carried out.

[0030] The heat-melting temperature of the resin in the above process (the temperature at which the heat-resistant release sheet 1 is used) is, for example, 150°C or higher, and may be 160°C or higher, 170°C or higher, or even 175°C or higher. However, the temperature at which the heat-resistant release sheet 1 is used is not limited to the above examples. Because the sheet contains a cutting sheet 2 made of PTFE or modified PTFE, which has excellent heat resistance, the temperature at which the sheet is used may be higher than the above examples, such as 200°C or higher, 250°C or higher, 275°C or higher, or even 300°C or higher.

[0031] [Method of carrying out a process involving heating and melting a resin] A process involving heat melting of a resin can be carried out using the heat-resistant release sheet 1. This method includes placing the heat-resistant release sheet 1 between the resin or an object containing the resin to be subjected to the process and a member that will come into contact with the resin or the object in the process, and carrying out the process while preventing direct contact between the resin or the object and the member using the sheet 1.

[0032] [Melt molding method] Resin can be melt-molded using heat-resistant release sheet 1. This melt-molding method involves placing heat-resistant release sheet 1 between a mold 12 and resin 13, and melt-molding resin 13 while preventing direct contact between mold 12 and resin 13 using sheet 1 (see FIG. 2).

[0033] [Method of manufacturing melt-molded product] A resin melt-molded product can be produced using the heat-resistant release sheet 1. The production method involves placing the heat-resistant release sheet 1 between a mold 12 and a resin 13, and melt-molding the resin 13 while preventing direct contact between the mold 12 and the resin 13 using the sheet 1 to obtain a resin melt-molded product (see FIG. 2).

[0034] [Heat and pressure treatment method] The object 35 can be subjected to a heat-pressure treatment using the heat-resistant release sheet 1. This heat-pressure treatment method is a method for heat-pressure treating the object 35 using a heat-pressure device, and includes placing the heat-resistant release sheet 1 between the object 35 and the heat-pressure surface 34, and performing the heat-pressure treatment while preventing direct contact between the object 35 and the heat-pressure surface 34 by the heat-resistant release sheet 1 (see FIG. 3).

[0035] [Method of manufacturing a heat-pressure treated product] A heat-pressure-treated product can be produced using the heat-resistant release sheet 1. This production method is a method for producing a heat-pressure-treated product using a heat-pressure device, and includes placing the heat-resistant release sheet 1 between an object 35 and a heat-pressure surface 34, and performing a heat-pressure treatment while preventing direct contact between the object 35 and the heat-pressure surface 34 using the sheet 1, to obtain a heat-pressure-treated product of the object 35. The heat-pressure treatment is, for example, heat-compression bonding or heat-pressing of the object 35, and in this case, a heat-pressure-bonded product or heat-pressed product is obtained (see FIG. 3). [Example]

[0036] The present invention will be described in more detail below with reference to examples, but the present invention is not limited to the following examples.

[0037] First, the evaluation method for the heat-resistant release sheets produced in this example will be described.

[0038] Thickness The thickness was determined as the average value of measurements taken at any three points at 25°C using a digital micrometer (minimum division 0.001 mm).

[0039] [Dimensional shrinkage rate (175℃, 30 minutes)] The dimensional shrinkage caused by heating at 175°C for 30 minutes was evaluated as follows. First, the dimensions in the MD and TD directions (dimension X0 before heating) of the heat-resistant release sheet to be evaluated were measured. Next, the heat-resistant release sheet was placed in a heating bath and left to stand at 175°C for 30 minutes, then cooled to 25°C, and the dimensions in the MD and TD directions (dimension X1 after heating) were measured. From the measured dimensions X0 and X1, the dimensional shrinkage was calculated using the formula: (X0-X1) / X0×100(%). Calipers were used to measure the dimensions, and the maximum dimensions in each direction were taken as X0 and X1.

[0040] [Linear thermal expansion coefficient α (25-175℃)] The linear thermal expansion coefficient α in the temperature range of 25°C to 175°C was evaluated by the above-mentioned method using TMA. The evaluation was performed in both the MD and TD directions of the heat-resistant release sheet. The test specimens were rectangular, measuring 4 mm wide and 20 mm long, and five test specimens were used for the evaluation.

[0041] [Tensile strength and maximum tensile elongation] The tensile strength (tensile breaking strength) and maximum tensile elongation were determined by a tensile test using a tensile tester (AG-I, manufactured by Shimadzu Corporation). Evaluations were performed in both the MD and TD directions of the heat-resistant release sheet. The shape of the test piece was a dumbbell-shaped No. 3 (gauge length 20 mm) as specified in JIS K6251:1993. The measurement conditions were a measurement temperature of 25°C, a chuck distance of 35 mm, and a pulling speed of 200 mm / min. The maximum tensile elongation was calculated from the gauge length before the test and the gauge length at break.

[0042] [Whether or not there are wrinkles when setting the mold] The presence or absence of wrinkles when the mold was set was evaluated using a transfer molding device. The mold cavity was a rectangular parallelepiped with a width of 50 mm, a length of 50 mm, and a depth of 0.7 mm. A roll of heat-resistant release sheet processed into a strip shape with a width of 170 mm was set in the device, and the sheet was fed by conveying to a mold heated to 175°C and vacuum-adsorbed to the mold. The heat-resistant release sheet after vacuum adsorption was visually inspected for the presence or absence of wrinkles.

[0043] Example 1 PTFE powder (Polyflon PTFE M-18, manufactured by Daikin Industries, Ltd.) was introduced into a cylindrical mold and preformed under conditions of a temperature of 23°C, a pressure of 8.5 MPa, and a pressure application time of 1 hour. The formed preform was then removed from the mold and baked at 370°C for 24 hours to obtain a cylindrical PTFE block with a height of 300 mm and an outer diameter of 470 mm. The obtained PTFE block was then cut using a cutting lathe to obtain a cut PTFE sheet (thickness 55 μm, strip-shaped). The obtained cut sheet was then stretched in its width direction (TD) to obtain the heat-resistant release sheet (thickness 50 μm) of Example 1. A tenter stretching device was used to stretch the cut sheet, and the stretching temperature was 280°C and the stretch ratio was 1.1 times. The direction in which pressure was applied during preforming was the TD direction of the obtained sheet.

[0044] Example 2 A modified PTFE cut sheet (thickness 55 μm, strip-like) was obtained in the same manner as in Example 1, except that modified PTFE powder (manufactured by 3M, Dyneon TFM modified PTFE TFM1700, TFE unit content 99% by mass or more) was used instead of PTFE powder. Next, the obtained cut sheet was stretched in its width direction (TD direction) to obtain a heat-resistant release sheet (thickness 51 μm) of Example 2. The stretching method and conditions were the same as in Example 1.

[0045] Example 3 The heat-resistant release sheet of Example 3 (thickness 49 μm) was obtained in the same manner as in Example 2, except that the cutting thickness was changed so that the thickness of the cut sheet before stretching was 70 μm and the stretching ratio was 1.2 times.

[0046] (Comparative Example 1) A 50 μm thick cut PTFE sheet was obtained in the same manner as in Example 1, except that the cutting thickness was changed. This was used as the heat-resistant release sheet of Comparative Example 1 without being stretched in the width direction.

[0047] (Comparative Example 2) A modified PTFE cut sheet having a thickness of 50 μm was obtained in the same manner as in Example 2, except that the cutting thickness was changed. This was used as the heat-resistant release sheet of Comparative Example 2 without being stretched in the width direction.

[0048] The evaluation results are summarized in Table 1 below.

[0049] [Table 1]

[0050] As shown in Table 1, in the heat-resistant release sheets of the comparative examples, which had a negative dimensional shrinkage rate in the TD direction, streaky wrinkles extending in the MD direction occurred when the sheets were set in the mold, but in the heat-resistant release sheets of the examples, which had dimensional shrinkage rates of more than 0% in both the MD and TD directions, no wrinkles occurred in either direction. [Industrial Applicability]

[0051] The heat-resistant release sheet of the present invention can be used in processes involving heat melting of resins. Examples of such processes include melt molding of resins using a mold and heat and pressure treatment of resin-containing objects using a heat and pressure device. [Explanation of symbols]

[0052] 1. Heat-resistant release sheet 2 Cutting Sheet

Claims

1. A heat-resistant release sheet that is disposed between a resin or an object containing the resin and a member that comes into contact with the resin or the object in a process involving heat melting of the resin, to prevent direct contact between the resin or the object and the member, when the resin or the object is subjected to the process involving heat melting of the resin, It comprises a cutting sheet of polytetrafluoroethylene (PTFE) or modified PTFE, the content of tetrafluoroethylene (TFE) units in the modified PTFE is 99% by mass or more, The dimensional shrinkage rate caused by heating at 175°C for 30 minutes exceeds 0% in each of two mutually perpendicular in-plane directions of the heat-resistant release sheet, The heat-resistant release sheet, wherein the two directions are the MD direction and the TD direction of the cut sheet.

2. 2. The heat-resistant release sheet according to claim 1, wherein the difference between the dimensional shrinkage rates in each of the two directions is less than 5.0%.

3. The linear thermal expansion coefficient in the temperature range from 25°C to 175°C is 150 x 10 for each of the two directions. -6 The heat-resistant release sheet according to claim 1 or 2, wherein the temperature is 100°C or lower.

4. 4. The heat-resistant release sheet according to claim 1, wherein the tensile strength is 30 MPa or more and the maximum tensile elongation is 250% or more in each of the two directions.

5. A method for carrying out a process involving heating and melting a resin, a heat-resistant release sheet is placed between the resin or an object containing the resin to be subjected to the process and a member that comes into contact with the resin or the object in the process, and the process is carried out in a state where the heat-resistant release sheet prevents direct contact between the resin or the object and the member, The heat-resistant release sheet according to any one of claims 1 to 4,

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