CN111574794B - High-dielectric-constant polytetrafluoroethylene film and preparation method and application thereof - Google Patents
High-dielectric-constant polytetrafluoroethylene film and preparation method and application thereof Download PDFInfo
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- -1 polytetrafluoroethylene Polymers 0.000 title claims abstract description 93
- 229920001343 polytetrafluoroethylene Polymers 0.000 title claims abstract description 93
- 239000004810 polytetrafluoroethylene Substances 0.000 title claims abstract description 93
- 238000002360 preparation method Methods 0.000 title claims abstract description 44
- 239000000843 powder Substances 0.000 claims abstract description 114
- 239000000463 material Substances 0.000 claims abstract description 69
- 229910010252 TiO3 Inorganic materials 0.000 claims abstract description 59
- 239000002994 raw material Substances 0.000 claims abstract description 34
- 239000000919 ceramic Substances 0.000 claims abstract description 15
- 239000008204 material by function Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims description 67
- 238000000498 ball milling Methods 0.000 claims description 39
- 238000005245 sintering Methods 0.000 claims description 25
- 238000003825 pressing Methods 0.000 claims description 16
- 238000005520 cutting process Methods 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 11
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 5
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 3
- 229910002370 SrTiO3 Inorganic materials 0.000 claims description 3
- 238000007723 die pressing method Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 claims 6
- 238000000465 moulding Methods 0.000 claims 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims 1
- 238000004891 communication Methods 0.000 abstract description 6
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical class [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 abstract description 3
- 238000007689 inspection Methods 0.000 abstract description 3
- 239000010936 titanium Substances 0.000 description 49
- 238000010438 heat treatment Methods 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 2
- 229920006362 Teflon® Polymers 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- 239000011863 silicon-based powder Substances 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000007655 standard test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
- C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
- C04B35/465—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates
- C04B35/468—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3293—Tin oxides, stannates or oxide forming salts thereof, e.g. indium tin oxide [ITO]
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- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
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Abstract
The invention discloses a high dielectric constant polytetrafluoroethylene film and a preparation method and application thereof, wherein the high dielectric constant polytetrafluoroethylene film is prepared by putting raw materials comprising polytetrafluoroethylene and functional materials, and the functional materials comprise (Ba)1‑xSrx)TiO3And Ba (Ti)1‑ySny)O3Wherein x is 0.3-0.6, and y is 0.1-0.2. In the invention, in order to modify the dielectric property of the polytetrafluoroethylene material, two kinds of modified barium titanate ceramic fine powder are added into the polytetrafluoroethylene as functional materials; through inspection, under the high frequency of 10GHz, the dielectric constant of the polytetrafluoroethylene film is adjustable between 2.3 and 80, and the dielectric loss is lower than 1.0 multiplied by 10‑3And the requirements of different designs in the field of 5G communication can be met.
Description
Technical Field
The invention belongs to the technical field of 5G communication, and particularly relates to a high-dielectric-constant polytetrafluoroethylene film, and a preparation method and application thereof.
Background
The trend in development of electronic information products and devices is toward higher frequencies and miniaturization, while organic materials having a high dielectric constant are advantageous for miniaturization and miniaturization of electronic devices.
Under high frequency transmission, polytetrafluoroethylene materials are the best performing organic materials discovered so far. The polytetrafluoroethylene has good dielectric property, excellent high temperature resistance and natural V0-grade flame retardant property. However, the teflon material has limitations, such as low dielectric constant (about 2.4-2.9) of pure teflon material, which limits its wide application in high frequency PCB board in 5G communication field.
In order to solve the problems, the Chinese patent application with the publication number of CN 107775975A discloses a high-dielectric constant broad-width polytetrafluoroethylene functional film and a manufacturing process thereof, wherein the polytetrafluoroethylene functional film is formed by turning or rotary cutting a polytetrafluoroethylene blank added with nano-scale high-purity superfine silicon powder or titanium dioxide. Under the high frequency of 10G-30G Hz, the dielectric constant of the polytetrafluoroethylene functional film is between 2.5 and 20 and depends on the addition amount (between 2 and 20 percent) of the functional material (namely the nano-grade high-purity superfine silicon powder or titanium dioxide).
The dielectric constant of the polytetrafluoroethylene functional film is adjustable, and the film with the required dielectric constant property can be prepared according to actual needs. But the adjustable range is still narrow, and the specific application scene is limited.
Disclosure of Invention
The invention aims to provide a polytetrafluoroethylene film with a high dielectric constant, and a preparation method and application thereof.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the high dielectric constant polytetrafluoroethylene film comprises polytetrafluoroethylene and a functional material, wherein the functional material is (Ba)1-xSrx)TiO3And Ba (Ti)1-ySny)O3Wherein x is 0.3-0.6, and y is 0.1-0.2.
In the invention, in order to modify the dielectric property of the polytetrafluoroethylene material, two kinds of modified barium titanate ceramic fine powder are added into the polytetrafluoroethylene as functional materials; through inspection, under the high frequency of 10GHz, the dielectric constant of the polytetrafluoroethylene film is adjustable between 2.3 and 80, and the dielectric loss is lower than 1.0 multiplied by 10-3And the requirements of different designs in the field of 5G communication can be met.
In the above-mentioned high dielectric constant polytetrafluoroethylene film, said functional material is composed of (Ba)1-xSrx)TiO3And Ba (Ti)1-ySny)O3The composition is shown in the specification, wherein x is 0.5, and y is 0.13.
In the above-mentioned high dielectric constant polytetrafluoroethylene film, among the functional materials, (Ba)1-xSrx)TiO3And Ba (Ti)1-ySny)O3The mass ratio of (1) to (0.1-10).
In the high dielectric constant polytetrafluoroethylene film, the mass ratio of the functional material to the polytetrafluoroethylene is (0.5-10): 1000.
the preparation method of the high dielectric constant polytetrafluoroethylene film comprises the following steps:
(1) preparation (Ba)1-xSrx)TiO3Fine powder and Ba (Ti)1-ySny)O3Fine powder, and mixing (Ba) according to a preset mass ratio1- xSrx)TiO3Fine powder and Ba (Ti)1-ySny)O3Mixing the fine powder into functional materialFeeding;
(2) uniformly mixing the functional material and the polytetrafluoroethylene fine powder according to a preset mass ratio to obtain a mixed raw material;
(3) preparing the mixed raw materials into a blank by a mould pressing method, and sintering the blank into a blank;
(4) and turning or rotary-cutting the blank into the high-dielectric-constant polytetrafluoroethylene film according to the preset film thickness.
In the above-mentioned preparation method of the high dielectric constant polytetrafluoroethylene film, in the step (1), (Ba)1-xSrx)TiO3The preparation method of the fine powder comprises the following steps:
(1.1) accurately weighing BaTiO according to the chemical formula3、SrTiO3And TiO2Uniformly mixing, carrying out primary ball milling, drying after ball milling, and sieving by a 40-mesh sieve to obtain a primary ball grinding material;
(1.2) pre-burning the primary ball-milling material at the temperature of 1000-1100 ℃ for 2.5-3.5h, and then carrying out secondary ball-milling to obtain a secondary ball-milling material;
(1.3) adding a binder into the secondary ball-milling material, uniformly mixing, preparing a blank by a die pressing method, and sintering the blank into (Ba)1-xSrx)TiO3A ceramic;
(1.4) adding said (Ba)1-xSrx)TiO3Ball milling the ceramic, drying to obtain Ba with particle size of 1-50 μm1-xSrx)TiO3And (3) fine powder.
Preferably, (Ba)1-xSrx)TiO3The particle size of the fine powder is 5-35 μm.
In the above-mentioned preparation method of the high dielectric constant polytetrafluoroethylene film, in the step (1), Ba (Ti)1-ySny)O3The preparation method of the fine powder comprises the following steps:
(1.5) accurately weighing BaTiO according to the chemical formula3、SnO2And TiO2Uniformly mixing, carrying out primary ball milling, drying after ball milling, and sieving by a 40-mesh sieve to obtain a primary ball grinding material;
(1.6) pre-burning the primary ball-milling material at the temperature of 1000-1100 ℃ for 2.5-3.5h, and then carrying out secondary ball-milling to obtain a secondary ball-milling material;
(1.7) adding a binder into the secondary ball-milling material, uniformly mixing, preparing a blank by a die pressing method, and sintering the blank into Ba (Ti)1-ySny)O3A ceramic;
(1.8) reacting said Ba (Ti)1-ySny)O3Ball milling the ceramic, drying to obtain Ba (Ti) with particle size of 1-50 μm1-ySny)O3And (3) fine powder.
Preferably, Ba (Ti)1-ySny)O3The particle size of the fine powder is 5-35 μm.
In the preparation method of the polytetrafluoroethylene film with the high dielectric constant, in the step (2), the functional material and the polytetrafluoroethylene fine powder are uniformly mixed for 0.5-5h at the speed of 100-3000 r/min.
Preferably, in the above preparation method of the polytetrafluoroethylene film with high dielectric constant, in the step (2), the functional material and the polytetrafluoroethylene fine powder are mixed uniformly at 500-1500r/min for 1-4 h.
In the preparation method of the polytetrafluoroethylene film with the high dielectric constant, in the step (3), the mixed raw materials are placed under the pressure of 5-100MPa and pressed for 1-10 h; and sintering the blank at the temperature of 320-450 ℃ for 5-150 h.
Preferably, in the preparation method of the polytetrafluoroethylene film with the high dielectric constant, in the step (3), the mixed raw materials are placed under 10-50MPa and pressed for 2-6 h; and sintering the blank at the temperature of 330-380 ℃ for 10-80 h.
The high dielectric constant polytetrafluoroethylene film prepared by the invention can be processed into a film with the width of 10-1700mm and the thickness of 0.01-5mm according to actual needs.
The invention also provides the application of the high-dielectric-constant polytetrafluoroethylene film in 5G communication.
Compared with the prior art, the invention has the beneficial effects that:
in the high dielectric constant polytetrafluoroethylene film of the invention, two kinds of modified barium titanate ceramic fine powder are added into polytetrafluoroethylene as functionsA material to modify the dielectric properties of the polytetrafluoroethylene material; through inspection, under the high frequency of 10-30GHz, the dielectric constant of the polytetrafluoroethylene film is adjustable between 2.3-80, and the dielectric loss is lower than 1.0 multiplied by 10-3And the requirements of different designs in the field of 5G communication can be met.
Detailed Description
The technical means of the present invention will be described in further detail below with reference to specific embodiments.
Example 1
The preparation method of the high dielectric constant polytetrafluoroethylene film comprises the following steps:
(1) preparation (Ba)1-xSrx)TiO3Fine powder and Ba (Ti)1-ySny)O3Fine powder, and mixing (Ba) according to the mass ratio of 1:0.11- xSrx)TiO3Fine powder and Ba (Ti)1-ySny)O3Mixing the fine powder into a functional material;
wherein x is 0.3 and y is 0.2;
specifically, (Ba)1-xSrx)TiO3The preparation method of the fine powder comprises the following steps:
(1.1) accurately weighing BaTiO according to the chemical formula3、SrTiO3And TiO2Uniformly mixing, putting into a ball milling tank, introducing deionized water as a ball milling medium, and carrying out primary ball milling for 6 hours; after ball milling, putting the mixture into an oven for drying and sieving the mixture by a 40-mesh sieve to obtain a primary ball grinding material;
(1.2) putting the primary ball grinding material into a crucible, presintering for 3h at 1000 ℃, then carrying out secondary ball milling for 6h in a ball mill, discharging and drying again to obtain a secondary ball grinding material;
(1.3) adding 8% of binder PVA into the secondary ball-milled material, uniformly mixing, sieving and granulating, pressing the powder into a proper cylindrical blank by using a tablet press, sintering the blank in a sintering furnace at the heating rate of 5 ℃/min, keeping the temperature at 550 ℃ for 1h to discharge the PVA, then continuously heating to 1100-1175 ℃, and keeping the temperature for 6h to obtain (Ba)1-xSrx)TiO3A ceramic;
(1.4) mixing (Ba)1-xSrx)TiO3Ball milling the ceramic, drying to obtain (Ba) with particle size of 30 μm1-xSrx)TiO3And (3) fine powder.
Likewise, Ba (Ti)1-ySny)O3The preparation method of the fine powder comprises the following steps:
(1.5) accurately weighing BaTiO according to the formula3、SnO2And TiO2Uniformly mixing, putting into a ball milling tank, introducing deionized water as a ball milling medium, and carrying out primary ball milling for 6 hours; after ball milling, putting the mixture into an oven for drying and sieving the mixture by a 40-mesh sieve to obtain a primary ball grinding material;
(1.6) putting the primary ball grinding material into a crucible, presintering for 3h at 1000 ℃, then carrying out secondary ball milling for 6h in a ball mill, discharging and drying again to obtain a secondary ball grinding material;
(1.7) adding 8% of binder PVA into the secondary ball-milled material, uniformly mixing, sieving and granulating, pressing the powder into a proper cylindrical blank by using a tablet press, sintering the blank in a sintering furnace at the heating rate of 5 ℃/min, keeping the temperature at 550 ℃ for 1h to discharge the PVA, then continuously heating to 1100-1175 ℃, and keeping the temperature for 6h to obtain Ba (Ti)1-ySny)O3A ceramic;
(1.8) adding Ba (Ti)1-ySny)O3Ball milling the ceramic, drying to obtain Ba (Ti) with particle size of 20 μm1- ySny)O3And (3) fine powder.
(2) Mixing the functional material and the polytetrafluoroethylene fine powder according to the mass ratio of 0.5:1000, and uniformly mixing for 1h at 1000 r/min; obtaining a mixed raw material;
(3) pressing the mixed raw materials under 20MPa for 6h to prepare a cylindrical blank; sintering the blank at 350 ℃ for 30h to obtain a blank;
(4) turning or rotary cutting the blank into high dielectric constant polytetrafluoroethylene film with width of 1000mm and thickness of 0.5 mm.
Example 2
The preparation method of the high dielectric constant polytetrafluoroethylene film comprises the following steps:
(1) preparation (Ba)1-xSrx)TiO3Fine powder and Ba (Ti)1-ySny)O3Fine powder, and mixing (Ba) according to the mass ratio of 1:11-xSrx)TiO3Fine powder and Ba (Ti)1-ySny)O3Mixing the fine powder into a functional material;
wherein x is 0.4 and y is 0.16;
(Ba1-xSrx)TiO3fine powder and Ba (Ti)1-ySny)O3The fine powder was prepared in the same manner as in example 1;
(2) mixing the functional material and the polytetrafluoroethylene fine powder according to the mass ratio of 2:1000, and uniformly mixing for 2 hours at 800 r/min; obtaining a mixed raw material;
(3) pressing the mixed raw materials under 30MPa for 5h to prepare a cylindrical blank; sintering the blank at 380 deg.c for 20 hr to form blank;
(4) turning or rotary cutting the blank into high dielectric constant polytetrafluoroethylene film with width of 1000mm and thickness of 0.5 mm.
Example 3
The preparation method of the high dielectric constant polytetrafluoroethylene film comprises the following steps:
(1) preparation (Ba)1-xSrx)TiO3Fine powder and Ba (Ti)1-ySny)O3Fine powder, and mixing (Ba) according to the mass ratio of 1:51-xSrx)TiO3Fine powder and Ba (Ti)1-ySny)O3Mixing the fine powder into a functional material;
wherein x is 0.5 and y is 0.13;
(Ba1-xSrx)TiO3fine powder and Ba (Ti)1-ySny)O3The fine powder was prepared in the same manner as in example 1;
(2) mixing the functional material and the polytetrafluoroethylene fine powder according to the mass ratio of 5:1000, and uniformly mixing for 4 hours at 500 r/min; obtaining a mixed raw material;
(3) pressing the mixed raw materials under 10MPa for 6h to prepare a cylindrical blank; sintering the blank at 360 ℃ for 15h to obtain a blank;
(4) turning or rotary cutting the blank into high dielectric constant polytetrafluoroethylene film with width of 1000mm and thickness of 0.5 mm.
Example 4
The preparation method of the high dielectric constant polytetrafluoroethylene film comprises the following steps:
(1) preparation (Ba)1-xSrx)TiO3Fine powder and Ba (Ti)1-ySny)O3Fine powder, and mixing (Ba) according to the mass ratio of 1:101- xSrx)TiO3Fine powder and Ba (Ti)1-ySny)O3Mixing the fine powder into a functional material;
wherein x is 0.6 and y is 0.1;
(Ba1-xSrx)TiO3fine powder and Ba (Ti)1-ySny)O3The fine powder was prepared in the same manner as in example 1;
(2) mixing the functional material and the polytetrafluoroethylene fine powder according to the mass ratio of 10:1000, and uniformly mixing at 1500r/min for 0.5 h; obtaining a mixed raw material;
(3) pressing the mixed raw materials for 1h under 100MPa to prepare a cylindrical blank; sintering the blank at 450 ℃ for 5h to obtain a blank;
(4) turning or rotary cutting the blank into high dielectric constant polytetrafluoroethylene film with width of 1000mm and thickness of 0.5 mm.
Example 5
The preparation method of the high dielectric constant polytetrafluoroethylene film comprises the following steps:
(1) preparation (Ba)1-xSrx)TiO3Fine powder and Ba (Ti)1-ySny)O3Fine powder, and mixing (Ba) according to the mass ratio of 1:0.21- xSrx)TiO3Fine powder and Ba (Ti)1-ySny)O3Mixing the fine powder into a functional material;
wherein x is 0.6 and y is 0.2;
(Ba1-xSrx)TiO3fine powder and Ba (Ti)1-ySny)O3The fine powder was prepared in the same manner as in example 1;
(2) mixing the functional material and the polytetrafluoroethylene fine powder according to the mass ratio of 7:1000, and uniformly mixing for 1h at 2000 r/min; obtaining a mixed raw material;
(3) pressing the mixed raw materials under 5MPa for 10h to prepare a cylindrical blank; sintering the blank at 400 ℃ for 40h to obtain a blank;
(4) turning or rotary cutting the blank into high dielectric constant polytetrafluoroethylene film with width of 1000mm and thickness of 0.5 mm.
Example 6
The preparation method of the high dielectric constant polytetrafluoroethylene film comprises the following steps:
(1) preparation (Ba)1-xSrx)TiO3Fine powder and Ba (Ti)1-ySny)O3Fine powder, and mixing (Ba) according to the mass ratio of 1:0.41- xSrx)TiO3Fine powder and Ba (Ti)1-ySny)O3Mixing the fine powder into a functional material;
wherein x is 0.3 and y is 0.17;
(Ba1-xSrx)TiO3fine powder and Ba (Ti)1-ySny)O3The fine powder was prepared in the same manner as in example 1;
(2) mixing the functional material and the polytetrafluoroethylene fine powder according to the mass ratio of 3:1000, and uniformly mixing for 3 hours at the speed of 2500 r/min; obtaining a mixed raw material;
(3) pressing the mixed raw materials for 6 hours under 60MPa to prepare a cylindrical blank; sintering the blank at 350 ℃ for 25h to obtain a blank;
(4) turning or rotary cutting the blank into high dielectric constant polytetrafluoroethylene film with width of 1000mm and thickness of 0.5 mm.
Example 7
The preparation method of the high dielectric constant polytetrafluoroethylene film comprises the following steps:
(1) preparation (Ba)1-xSrx)TiO3Fine powder and Ba (Ti)1-ySny)O3The fine powder is obtained by grinding the raw materials,and mixing (Ba) in a mass ratio of 1:0.61- xSrx)TiO3Fine powder and Ba (Ti)1-ySny)O3Mixing the fine powder into a functional material;
wherein x is 0.4 and y is 0.2;
(Ba1-xSrx)TiO3fine powder and Ba (Ti)1-ySny)O3The fine powder was prepared in the same manner as in example 1;
(2) mixing the functional material and the polytetrafluoroethylene fine powder according to the mass ratio of 6:1000, and uniformly mixing at 3000r/min for 0.1 h; obtaining a mixed raw material;
(3) pressing the mixed raw materials for 1h under 80MPa to prepare a cylindrical blank; sintering the blank at 340 ℃ for 15h to obtain a blank;
(4) turning or rotary cutting the blank into high dielectric constant polytetrafluoroethylene film with width of 1000mm and thickness of 0.5 mm.
Example 8
The preparation method of the high dielectric constant polytetrafluoroethylene film comprises the following steps:
(1) preparation (Ba)1-xSrx)TiO3Fine powder and Ba (Ti)1-ySny)O3Fine powder, and mixing (Ba) according to the mass ratio of 1:0.81- xSrx)TiO3Fine powder and Ba (Ti)1-ySny)O3Mixing the fine powder into a functional material;
wherein x is 0.45 and y is 0.17;
(Ba1-xSrx)TiO3fine powder and Ba (Ti)1-ySny)O3The fine powder was prepared in the same manner as in example 1;
(2) mixing the functional material and the polytetrafluoroethylene fine powder according to the mass ratio of 2.5:1000, and uniformly mixing at 3000r/min for 0.1 h; obtaining a mixed raw material;
(3) pressing the mixed raw materials for 1h under 80MPa to prepare a cylindrical blank; sintering the blank at 340 ℃ for 15h to obtain a blank;
(4) turning or rotary cutting the blank into high dielectric constant polytetrafluoroethylene film with width of 1000mm and thickness of 0.5 mm.
Example 9
The preparation method of the high dielectric constant polytetrafluoroethylene film comprises the following steps:
(1) preparation (Ba)1-xSrx)TiO3Fine powder and Ba (Ti)1-ySny)O3Fine powder, and mixing (Ba) according to the mass ratio of 1:0.51- xSrx)TiO3Fine powder and Ba (Ti)1-ySny)O3Mixing the fine powder into a functional material;
wherein x is 0.51 and y is 0.11;
(Ba1-xSrx)TiO3fine powder and Ba (Ti)1-ySny)O3The fine powder was prepared in the same manner as in example 1;
(2) mixing the functional material and the polytetrafluoroethylene fine powder according to the mass ratio of 9:1000, and uniformly mixing at 3000r/min for 0.1 h; obtaining a mixed raw material;
(3) pressing the mixed raw materials for 1h under 80MPa to prepare a cylindrical blank; sintering the blank at 340 ℃ for 15h to obtain a blank;
(4) turning or rotary cutting the blank into high dielectric constant polytetrafluoroethylene film with width of 1000mm and thickness of 0.5 mm.
Example 10
The preparation method of the high dielectric constant polytetrafluoroethylene film comprises the following steps:
(1) preparation (Ba)1-xSrx)TiO3Fine powder and Ba (Ti)1-ySny)O3Fine powder, and mixing (Ba) according to the mass ratio of 1:21-xSrx)TiO3Fine powder and Ba (Ti)1-ySny)O3Mixing the fine powder into a functional material;
wherein x is 0.32 and y is 0.16;
(Ba1-xSrx)TiO3fine powder and Ba (Ti)1-ySny)O3The fine powder was prepared in the same manner as in example 1;
(2) mixing the functional material and the polytetrafluoroethylene fine powder according to the mass ratio of 5.5:1000, and uniformly mixing at 3000r/min for 0.1 h; obtaining a mixed raw material;
(3) pressing the mixed raw materials for 1h under 80MPa to prepare a cylindrical blank; sintering the blank at 340 ℃ for 15h to obtain a blank;
(4) turning or rotary cutting the blank into high dielectric constant polytetrafluoroethylene film with width of 1000mm and thickness of 0.5 mm.
Example 11
The preparation method of the high dielectric constant polytetrafluoroethylene film comprises the following steps:
(1) preparation (Ba)1-xSrx)TiO3Fine powder and Ba (Ti)1-ySny)O3Fine powder, and mixing (Ba) according to the mass ratio of 1:81-xSrx)TiO3Fine powder and Ba (Ti)1-ySny)O3Mixing the fine powder into a functional material;
wherein x is 0.38 and y is 0.13;
(Ba1-xSrx)TiO3fine powder and Ba (Ti)1-ySny)O3The fine powder was prepared in the same manner as in example 1;
(2) mixing the functional material and the polytetrafluoroethylene fine powder according to the mass ratio of 7.5:1000, and uniformly mixing at 3000r/min for 0.1 h; obtaining a mixed raw material;
(3) pressing the mixed raw materials for 1h under 80MPa to prepare a cylindrical blank; sintering the blank at 340 ℃ for 15h to obtain a blank;
(4) turning or rotary cutting the blank into high dielectric constant polytetrafluoroethylene film with width of 1000mm and thickness of 0.5 mm.
Example 12
The preparation method of the high dielectric constant polytetrafluoroethylene film comprises the following steps:
(1) preparation (Ba)1-xSrx)TiO3Fine powder and Ba (Ti)1-ySny)O3Fine powder, and mixing (Ba) according to the mass ratio of 1:71-xSrx)TiO3Fine powder and Ba (Ti)1-ySny)O3Mixing the fine powder into a functional material;
wherein x is 0.38 and y is 0.16;
(Ba1-xSrx)TiO3fine powder and Ba (Ti)1-ySny)O3The fine powder was prepared in the same manner as in example 1;
(2) mixing the functional material and the polytetrafluoroethylene fine powder according to the mass ratio of 4:1000, and uniformly mixing at 3000r/min for 0.1 h; obtaining a mixed raw material;
(3) pressing the mixed raw materials for 1h under 80MPa to prepare a cylindrical blank; sintering the blank at 340 ℃ for 15h to obtain a blank;
(4) turning or rotary cutting the blank into high dielectric constant polytetrafluoroethylene film with width of 1000mm and thickness of 0.5 mm.
The dielectric constant and dielectric loss of the polytetrafluoroethylene films prepared in examples 1 to 7 were measured at a test frequency of 10GHz according to the standard test method for dielectric constant (ASTM D150), and the results are shown in Table 1.
TABLE 1
| Numbering | Dielectric constant | Dielectric loss |
| Example 1 | 2.3 | 3.12×10-4 |
| Example 2 | 14.6 | 6.37×10-4 |
| Example 3 | 80.1 | 9.56×10-4 |
| Example 4 | 58.3 | 2.98×10-4 |
| Example 5 | 4.9 | 3.32×10-4 |
| Example 6 | 7.1 | 3.66×10-4 |
| Example 7 | 12.2 | 4.78×10-4 |
| Example 8 | 10.4 | 4.22×10-4 |
| Example 9 | 13.5 | 3.89×10-4 |
| Example 10 | 23.7 | 3.12×10-4 |
| Example 11 | 60.8 | 3.45×10-4 |
| Example 12 | 63.1 | 3.77×10-4 |
Claims (8)
1. The high dielectric constant polytetrafluoroethylene film is prepared from polytetrafluoroethylene and functional material, and is characterized in that the functional material is prepared from (Ba)1-xSrx)TiO3And Ba (Ti)1-ySny)O3Wherein x is 0.3-0.6, and y is 0.1-0.2;
among the functional materials, (Ba)1-xSrx)TiO3And Ba (Ti)1-ySny)O3The mass ratio of (1) to (0.1-10);
the mass ratio of the functional material to the polytetrafluoroethylene is (0.5-10): 1000.
2. the high dielectric constant polytetrafluoroethylene film according to claim 1 wherein said functional material is selected from the group consisting of (Ba)1-xSrx)TiO3And Ba (Ti)1-ySny)O3The composition is shown in the specification, wherein x is 0.5, and y is 0.13.
3. The method for preparing a high dielectric constant polytetrafluoroethylene film according to any of claims 1-2, comprising the steps of:
(1) preparation (Ba)1-xSrx)TiO3Fine powder and Ba (Ti)1-ySny)O3Fine powder, and mixing (Ba) according to a preset mass ratio1-xSrx)TiO3Fine powder and Ba (Ti)1-ySny)O3Mixing the fine powder into a functional material;
(2) uniformly mixing the functional material and the polytetrafluoroethylene fine powder according to a preset mass ratio to obtain a mixed raw material;
(3) preparing the mixed raw materials into a blank by a mould pressing method, and sintering the blank into a blank;
(4) and turning or rotary-cutting the blank into the high-dielectric-constant polytetrafluoroethylene film according to the preset film thickness.
4. The method for preparing a high dielectric constant polytetrafluoroethylene film according to claim 3, wherein in step (1), (Ba)1-xSrx)TiO3The preparation method of the fine powder comprises the following steps:
(1.1) accurately weighing BaTiO according to the chemical formula3、SrTiO3And TiO 22Uniformly mixing, carrying out primary ball milling, drying after ball milling, and sieving by a 40-mesh sieve to obtain a primary ball grinding material;
(1.2) pre-burning the primary ball-milling material at the temperature of 1000-1100 ℃ for 2.5-3.5h, and then carrying out secondary ball-milling to obtain a secondary ball-milling material;
(1.3) adding a binder into the secondary ball-milling material, uniformly mixing, preparing a blank by a die pressing method, and sintering the blank into (Ba)1-xSrx)TiO3A ceramic;
(1.4) adding said (Ba)1-xSrx)TiO3Ball milling the ceramic, drying to obtain Ba with particle size of 1-50 μm1- xSrx)TiO3And (3) fine powder.
5. The method for preparing a high dielectric constant polytetrafluoroethylene film according to claim 3, wherein in step (1), Ba (Ti)1-ySny)O3The preparation method of the fine powder comprises the following steps:
(1.5) accurately weighing BaTiO according to the chemical formula3、SnO2And TiO2Uniformly mixing, carrying out primary ball milling, drying after ball milling, and sieving by a 40-mesh sieve to obtain a primary ball grinding material;
(1.6) pre-burning the primary ball-milling material at the temperature of 1000-1100 ℃ for 2.5-3.5h, and then carrying out secondary ball-milling to obtain a secondary ball-milling material;
(1.7) in the secondary ball millingAdding binder into the raw materials, mixing, making into blank by molding method, and sintering the blank into Ba (Ti)1-ySny)O3A ceramic;
(1.8) reacting said Ba (Ti)1-ySny)O3Ball milling the ceramic, drying to obtain Ba (Ti) with particle size of 1-50 μm1-ySny)O3And (3) fine powder.
6. The method for preparing the polytetrafluoroethylene film with high dielectric constant as claimed in claim 3, wherein in the step (2), the functional material and the polytetrafluoroethylene fine powder are mixed uniformly for 0.5-5h at 3000 r/min.
7. The method for preparing a high dielectric constant polytetrafluoroethylene film according to claim 3, wherein in the step (3), the mixed raw materials are pressed for 1 to 10 hours under a pressure of 5 to 100 MPa; and sintering the blank at the temperature of 320-450 ℃ for 5-150 h.
8. Use of the high dielectric constant polytetrafluoroethylene film according to any of claims 1-2 in 5G telecommunications.
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