CN111823619A - Preparation method of PTFE composite material film, PTFE film and copper-clad plate using PTFE film - Google Patents
Preparation method of PTFE composite material film, PTFE film and copper-clad plate using PTFE film Download PDFInfo
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- CN111823619A CN111823619A CN202010590100.XA CN202010590100A CN111823619A CN 111823619 A CN111823619 A CN 111823619A CN 202010590100 A CN202010590100 A CN 202010590100A CN 111823619 A CN111823619 A CN 111823619A
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- 229920001343 polytetrafluoroethylene Polymers 0.000 title claims abstract description 67
- 239000004810 polytetrafluoroethylene Substances 0.000 title claims abstract description 67
- 239000002131 composite material Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 54
- 238000003825 pressing Methods 0.000 claims abstract description 38
- 238000005245 sintering Methods 0.000 claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 16
- 239000011256 inorganic filler Substances 0.000 claims abstract description 14
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 14
- 239000011347 resin Substances 0.000 claims abstract description 14
- 229920005989 resin Polymers 0.000 claims abstract description 14
- 239000000725 suspension Substances 0.000 claims abstract description 12
- 238000005520 cutting process Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 239000000377 silicon dioxide Substances 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 229910052681 coesite Inorganic materials 0.000 claims description 5
- 229910052906 cristobalite Inorganic materials 0.000 claims description 5
- 229910052682 stishovite Inorganic materials 0.000 claims description 5
- 229910052905 tridymite Inorganic materials 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 239000012528 membrane Substances 0.000 claims 1
- -1 Polytetrafluoroethylene Polymers 0.000 description 6
- 239000000843 powder Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001739 density measurement Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D7/00—Producing flat articles, e.g. films or sheets
- B29D7/01—Films or sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/006—Pressing and sintering powders, granules or fibres
-
- 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
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
- B32B15/085—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin comprising polyolefins
-
- 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
- B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
-
- 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
- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
- B32B27/20—Layered products comprising a layer of synthetic resin characterised by the use of special additives using fillers, pigments, thixotroping agents
-
- 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
- B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
- B32B27/322—Layered products comprising a layer of synthetic resin comprising polyolefins comprising halogenated polyolefins, e.g. PTFE
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2027/00—Use of polyvinylhalogenides or derivatives thereof as moulding material
- B29K2027/12—Use of polyvinylhalogenides or derivatives thereof as moulding material containing fluorine
- B29K2027/18—PTFE, i.e. polytetrafluorethene, e.g. ePTFE, i.e. expanded polytetrafluorethene
-
- 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
- B32B2250/00—Layers arrangement
- B32B2250/40—Symmetrical or sandwich layers, e.g. ABA, ABCBA, ABCCBA
-
- 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
- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
- B32B2307/72—Density
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Casting Or Compression Moulding Of Plastics Or The Like (AREA)
Abstract
The invention discloses a preparation method of a PTFE composite material film, which comprises the following steps: (1) uniformly mixing PTFE suspension resin and an inorganic filler to obtain a mixture; (2) providing a mould with a cavity with the depth H, filling 1/3H of mixture into the cavity with P1Pressure pressing and holding pressure t1Time; then to the cavityThe mixture with the depth of 1/3H is filled in the container, and the mixture is filled with P2Pressure pressing and holding pressure t2Time; finally, filling the cavity with the mixture, and filling the cavity with P3Pressure pressing and holding pressure t3Time, obtaining a preform in which P1<P2<P3(ii) a (3) Sintering the blank in the die; (4) and cutting the sintered material into a PTEF composite material film. The invention also discloses the PTFE composite material film prepared by the method and a copper-clad plate using the PTFE composite material film. The preparation method of the invention improves the density uniformity of the PTFE composite film produced in each batch.
Description
Technical Field
The invention relates to the field of copper-clad plates, in particular to a preparation method of a PTFE composite material film, a PTFE film and a copper-clad plate applying the PTFE film.
Background
Polytetrafluoroethylene (PTFE) has excellent dielectric properties, chemical resistance, heat resistance, flame retardancy, small dielectric constant and dielectric loss and small variation in a high frequency range, but is molded by a method such as molding and sintering because of its high viscosity in a molten state. The polytetrafluoroethylene has large expansion coefficient, soft texture, small bending strength and poor mechanical property, and the common method for overcoming the defects of the polytetrafluoroethylene is to modify the polytetrafluoroethylene by using inorganic filler. Pressing the mixture of the polytetrafluoroethylene and the inorganic filler into a blank, sintering the blank into a material block, and turning the material block into a film. The pressing process of the polytetrafluoroethylene and inorganic filler mixture has a great influence on the uniformity of the density of the sintered material. In the conventional pressing method, internal friction between the particles and external friction between the particles and the inner wall of the cavity hinder the transmission of pressure when the particles are rearranged, so that the lower layer has a lower degree of compaction than the upper layer, resulting in a difference in density of the same batch of PTFE composite film products.
Disclosure of Invention
In order to solve the above problems of the prior art, the present invention provides a method for preparing a PTFE composite film, comprising the steps of:
(1) uniformly mixing PTFE suspension resin and an inorganic filler to obtain a mixture;
(2) providing a mould with a cavity with the depth H, filling 1/3H of mixture into the cavity with P1Pressure pressing and holding pressure t1Time; then the mould cavity is filled with the mixture with the depth of 1/3H to P2Pressure pressing and holding pressure t2Time; finally, filling the cavity with the mixture, and filling the cavity with P3Pressure pressing and holding pressure t3Time, obtaining a preform in which P1<P2<P3；
(3) Sintering the blank in the die;
(4) and cutting the sintered material into a PTEF composite material film.
In some embodiments, the depth of the mold is 1800-1＝5MPa，P2＝10MPa，P3＝20MPa。
In certain embodiments, t1Is 3-5min, t2Is 3-5min, t3Is 30-35 min.
In certain embodiments, the PTFE suspending resin has a particle size of no more than 200 μm and a molecular weight of from 100 to 800 ten thousand.
In some embodiments, the sintering temperature is 370-390 ℃ and the sintering time is 5-6 days.
In certain embodiments, the PTFE suspension resin comprises 55-60% and the inorganic filler comprises 40-55% by weight of the blend.
The invention also discloses a PTFE composite material film prepared by the preparation method of the PTFE composite material film, wherein the inorganic filler is SiO2The thickness of the PTFE film is 0.5-2 mm.
The invention also discloses a copper-clad plate using the PTFE composite material film, which comprises the PTFE composite material film and copper plates attached to two sides of the PTFE composite material film.
The invention has the beneficial effects that: the density uniformity of the PTFE composite film produced in each batch is improved.
Drawings
Fig. 1 is a flowchart of a method for producing a PTFE composite film according to an embodiment of the present invention.
FIG. 2 is a schematic view of a density measurement sampling position of a material obtained by sintering.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
Referring to fig. 1, a method for preparing a PTFE composite film includes the following steps:
(1) uniformly mixing PTFE suspension resin and an inorganic filler to obtain a mixture;
(2) providing a mould with a cavity with the depth H, filling 1/3H of mixture into the cavity with P1Pressure pressing and holding pressure t1Time; then the mould cavity is filled with the mixture with the depth of 1/3H to P2Pressure pressing and holding pressure t2Time; finally, filling the cavity with the mixture, and filling the cavity with P3Pressure pressing and holding pressure t3Time, obtaining a preform in which P1<P2<P3；
(3) Sintering the blank in the die;
(4) and cutting the sintered material into a PTEF composite material film.
In some embodiments, the depth of the mold is 1800-1＝5MPa，P2＝10MPa，P3＝20MPa。
In certain embodiments, t1Is 3-5min, t2Is 3-5min, t3Is 30-35 min.
In certain embodiments, the PTFE suspending resin has a particle size of no more than 200 μm and a molecular weight of from 100 to 800 ten thousand.
In some embodiments, the sintering temperature is 370-390 ℃ and the sintering time is 5-6 days.
In certain embodiments, the PTFE suspension resin comprises 55-60% and the inorganic filler comprises 40-55% by weight of the blend.
The invention also discloses a PTFE composite material film prepared by the preparation method of the PTFE composite material film, wherein the inorganic filler is SiO2The thickness of the PTFE film is 0.5-2 mm.
The invention also discloses a copper-clad plate using the PTFE composite material film, which comprises the PTFE composite material film and copper plates attached to two sides of the PTFE composite material film.
Example 1
55 parts of PTFE suspension resin having a particle size of not more than 200 μm and 45 parts of silica powder having a particle size of not more than 30 μm were mixed uniformly. And pressing the mixture by adopting a die with a cavity depth of 1800 mm. Firstly, filling the mixture into a mold, paving and compacting the mixture, wherein the filling height of the mixture is 60mm, and then applying pressure of 5MPa for first pressing, and the pressure maintaining time is 3-5 min. And then, filling the mixture into the mold, paving and compacting the mixture, wherein the filling height of the mixture is 60mm, and then applying the pressure of 10MPa for secondary pressing, wherein the pressure maintaining time is 3-5 min. And finally, filling the mixture into the mold, paving and compacting the mixture to fill the cavity with the mixture, and pressing at the pressure of 20MPa for 30-35 min.
And after the pressing is finished, taking out the obtained blank, and sintering the blank in a sintering furnace. The sintering temperature is controlled at 370 ℃ and 390 ℃, and the sintering time is 5-6 days. And cutting the sintered material into a PTEF composite film.
Example 2
60 parts of PTFE suspension resin having a particle size of not more than 200 μm and 40 parts of silica powder having a particle size of not more than 30 μm were mixed uniformly. And pressing the mixture by adopting a die with a cavity depth of 2000 mm. Firstly, filling the mixture into a mold, paving and compacting the mixture, wherein the filling height of the mixture is 66-67mm, and then applying the pressure of 5MPa for first pressing, and the pressure maintaining time is 3-5 min. And then, filling the mixture into the mold, paving and compacting the mixture, wherein the filling height of the mixture is 66-67mm, and then applying the pressure of 10MPa for second pressing, wherein the pressure maintaining time is 3-5 min. And finally, filling the mixture into the mold, paving and compacting the mixture to fill the cavity with the mixture, and pressing at the pressure of 20MPa for 30-35 min.
And after the pressing is finished, taking out the obtained blank, and sintering the blank in a sintering furnace. The sintering temperature is controlled at 370 ℃ and 390 ℃, and the sintering time is 5-6 days. And cutting the sintered material into a PTEF composite film.
Example 3
60 parts of PTFE suspension resin having a particle size of not more than 200 μm and 40 parts of silica powder having a particle size of not more than 30 μm were mixed uniformly. And pressing the mixture by adopting a die with a cavity depth of 2100 mm. Firstly, filling the mixture into a mold, paving and compacting the mixture, wherein the filling height of the mixture is 70mm, and then applying pressure of 5MPa for first pressing, and the pressure maintaining time is 3-5 min. And then, filling the mixture into the mold, paving and compacting the mixture, wherein the filling height of the mixture is 70mm, and then applying the pressure of 10MPa for secondary pressing, wherein the pressure maintaining time is 3-5 min. And finally, filling the mixture into the mold, paving and compacting the mixture to fill the cavity with the mixture, and pressing at the pressure of 20MPa for 30-35 min.
And after the pressing is finished, taking out the obtained blank, and sintering the blank in a sintering furnace. The sintering temperature is controlled at 370 ℃ and 390 ℃, and the sintering time is 5-6 days. And cutting the sintered material into a PTEF composite film.
Comparative examples
60 parts of PTFE suspension resin having a particle size of not more than 200 μm and 40 parts of silica powder having a particle size of not more than 30 μm were mixed uniformly. And pressing the mixture by adopting a die with a cavity depth of 2000 mm. And (3) putting the mixture into a mold once, and applying a pressure of 20MPa for 30-35 min. And after the pressing is finished, taking out the obtained blank, and sintering the blank in a sintering furnace. The sintering temperature is controlled at 370 ℃ and 390 ℃, and the sintering time is 5-6 days. And cutting the sintered material into a PTEF composite film.
The sintered materials of example 2 and comparative example were sampled from the upper, middle and lower three positions to measure the density. Example 2 the density of the sintered material at the upper, middle and lower three positions was 1.31g/cm3、1.31g/cm3And 1.30g/cm3While the density of the sintered material of comparative example was 1.31g/cm at the upper, middle and lower positions, respectively3、1.26g/cm3、1.23g/cm3. Compared with the traditional pressing method, the pressing method provided by the disclosure is filled for three times, and a pre-pressing procedure is respectively added after the first two times of filling, so that the uniformity of the material density is improved. In the conventional pressing method, in the granuleWhen the granules are rearranged, the internal friction between the granules and the external friction between the granules and the inner wall of the cavity hinder the transmission of pressure, so that the compactness of the lower layer is smaller than that of the upper layer.
The invention also discloses a PTFE composite material film prepared by the preparation method of the PTFE composite material film, wherein the inorganic filler is SiO2，SiO2The proportion of (A) is 40%
The invention also discloses a copper-clad plate using the PTFE composite material film, which comprises the PTFE composite material film and copper plates attached to two sides of the PTFE composite material film.
What has been described above are merely some embodiments of the present invention. It will be apparent to those skilled in the art that various changes and modifications can be made without departing from the inventive concept thereof, and these changes and modifications can be made without departing from the spirit and scope of the invention.
Claims (8)
- A method for producing a PTFE composite film, characterized by comprising the steps of:(1) uniformly mixing PTFE suspension resin and an inorganic filler to obtain a mixture;(2) providing a mould, wherein the mould is provided with a cavity with the depth H, and filling 1/3H of mixture into the cavity to P1Pressure pressing and holding pressure t1Time; then the mould cavity is filled with the mixture with the depth of 1/3H to P2Pressure pressing and holding pressure t2Time; finally, filling the cavity with the mixture, and filling the cavity with P3Pressure pressing and holding pressure t3Time, obtaining a preform in which P1<P2<P3；(3) Sintering the blank in the mold;(4) and cutting the sintered material into a PTEF composite material film.
- 2. The method for preparing a PTFE composite film according to claim 1, wherein the depth of the mold is H1800-2100 mm, P1＝5MPa，P2＝10MPa，P3＝20MPa。
- 3. The method for producing a PTFE composite film according to claim 2, characterized in that t is1Is 3-5min, t2Is 3-5min, t3Is 30-35 min.
- 4. The method for producing a PTFE composite film according to claim 1, characterized in that the PTFE suspension resin has a particle diameter of not more than 200 μm and a molecular weight of 100 to 800 ten thousand.
- 5. The method for producing a PTFE composite film according to claim 1, characterized in that the sintering temperature is 370-.
- 6. The method for producing a PTFE composite film according to claim 1, characterized in that in the mixture, the PTFE suspension resin is 55 to 60% by weight and the inorganic filler is 40 to 55% by weight.
- 7. A PTFE film produced by the production method of the PTFE composite film according to any one of claims 1 to 6, wherein the inorganic filler is SiO2And the thickness of the PTFE membrane is 0.5-2 mm.
- 8. The copper-clad plate using the PTFE composite film of claim 7, further comprising copper plates attached to both sides of the PTFE composite film.
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| CN202010590100.XA CN111823619A (en) | 2020-06-24 | 2020-06-24 | Preparation method of PTFE composite material film, PTFE film and copper-clad plate using PTFE film |
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Cited By (1)
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| US20220065737A1 (en) * | 2020-09-01 | 2022-03-03 | Beak Myeong SEONG | Liquid leak sensor and method of fabricating the same |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20220065737A1 (en) * | 2020-09-01 | 2022-03-03 | Beak Myeong SEONG | Liquid leak sensor and method of fabricating the same |
| US11747234B2 (en) * | 2020-09-01 | 2023-09-05 | Beak Myeong SEONG | Liquid leak sensor and method of fabricating the same |
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Application publication date: 20201027 |