CN115784744A - High-dielectric alloy composite film for high-frequency communication and preparation method thereof - Google Patents
High-dielectric alloy composite film for high-frequency communication and preparation method thereof Download PDFInfo
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Abstract
A high-dielectric alloy composite film for high-frequency communication and a preparation method thereof are disclosed, the high-dielectric alloy composite film is prepared by a high-dielectric blending agent and polytetrafluoroethylene suspension resin, wherein the high-dielectric blending agent is composed of the following raw materials in parts by mass: adopting 30-60 parts of strontium barium titanate powder, 7-17 parts of copper calcium titanate powder, 3-6 parts of zinc zirconate powder, 0.7-2.9 parts of bismuth titanate powder, 0.2-0.6 part of iron titanate powder, 0.5-1.2 parts of aluminum zirconate powder, 8-12 parts of magnesium titanate powder, 6-12 parts of silicon micropowder and 10-18 parts of titanium dioxide powder; and then carrying out primary drying, primary grinding, primary sieving, three-dimensional mixing, high-speed mixing, primary sintering, secondary grinding, secondary drying, secondary sieving, low-temperature high-speed mixing, pressing, secondary sintering, rotary cutting and slitting to finally obtain the polytetrafluoroethylene-based high-dielectric alloy composite membrane product. The polytetrafluoroethylene-based high-dielectric alloy composite film prepared by the invention has better performance consistency and can meet the application requirements.
Description
Technical Field
The invention relates to a high-dielectric alloy composite film for high-frequency communication and a preparation method thereof, belonging to the technical field of composite films.
Background
The trend of electronic information products and devices is toward high frequency, miniaturization, and the use of organic materials having a high dielectric constant is advantageous for miniaturization and miniaturization of electronic devices. High dielectric constant organic materials are greatly needed in the fields of 5G wireless networks, radars, beidou satellite communication and the like. Under high-frequency transmission, the polytetrafluoroethylene material is the best organic material found at present, has excellent insulating property, excellent temperature resistance and V0-level flame retardant property. However, the dielectric constant of pure PTFE is low, which limits its application in 5G communication field.
In the prior art, a method for preparing a polytetrafluoroethylene/ceramic composite membrane on the market is to impregnate polytetrafluoroethylene emulsion containing ceramic powder into glass fiber cloth, and then to dry the polytetrafluoroethylene emulsion to prepare the cloth. Because the surface polarity of the polytetrafluoroethylene emulsion is very low, and the surface polarity of the ceramic powder is higher and the density is larger than that of the emulsion, the ceramic powder is easy to precipitate in the dipping process and is easy to agglomerate in the drying process, so that the performance of the polytetrafluoroethylene-ceramic cloth is not uniform, the difference of the dielectric constant and the thermal expansion at different positions is large, and the application is influenced.
Disclosure of Invention
The invention provides a high-dielectric alloy composite film for high-frequency communication and a preparation method thereof, aiming at solving the problems in the background art, and the high-dielectric alloy composite film can ensure that the performance consistency of the composite film meets the application requirements.
The technical scheme for solving the technical problems is as follows: a high-dielectric alloy composite film for high-frequency communication is prepared from a high-dielectric blending agent and polytetrafluoroethylene suspension resin, wherein the high-dielectric blending agent is prepared from the following raw materials in parts by mass: 30-60 parts of strontium barium titanate powder, 7-17 parts of copper calcium titanate powder, 3-6 parts of zinc zirconate powder, 0.7-2.9 parts of bismuth titanate powder, 0.2-0.6 part of iron titanate powder, 0.5-1.2 parts of aluminum zirconate powder, 8-12 parts of magnesium titanate powder, 6-12 parts of silicon micropowder and 10-18 parts of titanium dioxide powder.
As a preferred scheme of the high-dielectric alloy composite film for high-frequency communication, the high-dielectric blending agent is composed of the following raw materials in parts by mass: 30 parts of strontium barium titanate powder, 7 parts of copper calcium titanate powder, 3 parts of zinc zirconate powder, 0.7 part of bismuth titanate powder, 0.2 part of iron titanate powder, 0.5 part of aluminum zirconate powder, 8 parts of magnesium titanate powder, 6 parts of silicon micropowder and 10 parts of titanium dioxide powder.
As a preferred scheme of the high-dielectric alloy composite film for high-frequency communication, the high-dielectric blending agent is composed of the following raw materials in parts by mass: 45 parts of strontium barium titanate powder, 12 parts of copper calcium titanate powder, 4.5 parts of zinc zirconate powder, 1.8 parts of bismuth titanate powder, 0.4 part of iron titanate powder, 0.8 part of aluminum zirconate powder, 10 parts of magnesium titanate powder, 9 parts of silicon micropowder and 14 parts of titanium dioxide powder.
As a preferred scheme of the high-dielectric alloy composite film for high-frequency communication, the high-dielectric blending agent is composed of the following raw materials in parts by mass: 60 parts of strontium barium titanate powder, 17 parts of copper calcium titanate powder, 6 parts of zinc zirconate powder, 2.9 parts of bismuth titanate powder, 0.6 part of iron titanate powder, 1.2 parts of aluminum zirconate powder, 12 parts of magnesium titanate powder, 12 parts of silicon micropowder and 18 parts of titanium dioxide powder.
The invention also provides a preparation method of the high-dielectric alloy composite film for high-frequency communication, which comprises the following steps:
(1) Preparing a high-dielectric blending agent:
(11) Primary drying: respectively placing barium strontium titanate powder, calcium copper titanate powder, zinc zirconate powder, bismuth titanate powder, iron titanate powder, aluminum zirconate powder, magnesium titanate powder, silicon micropowder and titanium dioxide powder in an electric heating oven, and continuously drying for 24-48h at 200 ℃;
(12) Primary grinding: grinding the materials after primary drying by adopting a planetary ball mill respectively, wherein hard alloy balls are adopted as grinding balls; the rotating speed of the ball mill is 200-400rpm; the diameter of the grinding ball is 5-15mm; ball material ratio: 2; grinding time: 5-50h;
(13) Primary sieving: sieving the materials after primary grinding by using an electric powder sieving machine respectively, wherein a sieve mesh is 180-325 meshes;
(14) Three-dimensional mixing: adding the materials after primary screening into three-dimensional mixing equipment according to a preset proportion, wherein the rotating speed of a main shaft of the three-dimensional mixing equipment is 10-15rpm, and the time is 1-6h;
(15) High-speed mixing: placing the three-dimensionally mixed materials in high-speed mixing equipment, wherein the rotating speed of a stirring paddle of the high-speed mixing equipment is 900-1440rpm, and the time is 0.5-4h;
(16) Primary sintering: placing the materials after high-speed mixing in a high-temperature sintering furnace, and continuously sintering for 48-72h at 450-1150 ℃;
(17) And (3) secondary grinding: grinding the primary sintered product by a planetary ball mill, wherein the grinding ball is a hard alloy ball; the rotating speed of the motor is as follows: 200-400rpm; grinding ball diameter: 5-15mm; ball material ratio: 2; grinding time: 5-50h;
(18) Secondary drying: continuously drying the materials subjected to secondary grinding for 24-48h at 200 ℃ by using an electric heating oven;
(19) And (3) secondary sieving: sieving the material after the secondary drying by using an electric powder sieving machine, wherein a sieve mesh is 300-350 meshes;
(2) Preparing a polytetrafluoroethylene-based high-dielectric alloy composite film:
(21) Low-temperature high-speed mixing: adding polytetrafluoroethylene resin and a high dielectric blending agent into mixing equipment with a cooling device according to the addition proportion, wherein the addition proportion of the high dielectric blending agent is 5-29%, and the rest proportion is added with the polytetrafluoroethylene resin; during mixing, the temperature of the cooling liquid is 2-7 ℃, and the rotating speed of a stirring paddle is 500-1100rpm;
(22) Pressing: adding the powder after low-temperature high-speed mixing into a hydraulic press die, adopting an up-down bidirectional simultaneous pressurization mode, keeping the pressure at 50-260MPa and the pressing speed at 3-15mm/min, keeping the pressure for at least 2h after a plunger stops moving, slowly reducing the pressure to 0, and ejecting a composite film blank;
(23) And (3) secondary sintering: placing the blank in a sintering furnace, closing a furnace door, slowly heating the sintering furnace from room temperature to 350-400 ℃, keeping the temperature for at least 20h, slowly cooling the temperature to room temperature, and taking out the composite film blank;
(24) Rotary cutting: fixing the composite film blank after secondary sintering on a mandrel, and enabling a turning tool to be parallel to the axis of the composite film blank to perform linear feeding motion;
(25) Slitting: and cutting the rotary-cut composite film blank into preset widths to obtain the polytetrafluoroethylene-based high-dielectric alloy composite film product.
As a preferred scheme of the preparation method of the high-dielectric alloy composite film for high-frequency communication, the step (21) comprises the following steps:
(211) Firstly, controlling the rotating speed of a stirring paddle at 500-700rpm for 5-15min;
(212) Then controlling the rotating speed of the stirring paddle at 900-1100rpm for 3-10min;
(213) Standing for 5-60min;
(214) Repeating the steps (211), (212) and (213) 3-8 times.
As a preferred scheme of the preparation method of the high-dielectric alloy composite membrane for high-frequency communication, in the step (21), polytetrafluoroethylene resin prepared by a suspension method is selected, and the particle size of the resin is 15-150 microns.
The beneficial effects of the invention are: the high-dielectric blending agent is prepared from a high-dielectric blending agent and polytetrafluoroethylene suspension resin, wherein the high-dielectric blending agent is prepared from the following raw materials in parts by mass: 30-60 parts of strontium barium titanate powder, 7-17 parts of copper calcium titanate powder, 3-6 parts of zinc zirconate powder, 0.7-2.9 parts of bismuth titanate powder, 0.2-0.6 part of iron titanate powder, 0.5-1.2 parts of aluminum zirconate powder, 8-12 parts of magnesium titanate powder, 6-12 parts of silicon micropowder and 10-18 parts of titanium dioxide powder are adopted; and then carrying out primary drying, primary grinding, primary sieving, three-dimensional mixing, high-speed mixing, primary sintering, secondary grinding, secondary drying, secondary sieving, low-temperature high-speed mixing, pressing, secondary sintering, rotary cutting and slitting to finally obtain the polytetrafluoroethylene-based high-dielectric alloy composite film product. According to the invention, the high dielectric powder is prepared and added into the polytetrafluoroethylene suspension resin, so that the prepared polytetrafluoroethylene-based high dielectric alloy composite membrane has good performance consistency, and the differences of dielectric constants and thermal expansion at different positions are small, so that the application requirements can be met.
Detailed Description
In order that the above objects, features and advantages of the present invention will be readily understood, numerous specific details are set forth in the following description in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Example 1:
the high-dielectric alloy composite film for high-frequency communication in example 1 is prepared from 29% of a high-dielectric blending agent and the balance of raw materials of polytetrafluoroethylene suspension resin, wherein the high-dielectric blending agent is composed of the following raw materials in parts by mass: 30 parts of strontium barium titanate powder, 7 parts of copper calcium titanate powder, 3 parts of zinc zirconate powder, 0.7 part of bismuth titanate powder, 0.2 part of iron titanate powder, 0.5 part of aluminum zirconate powder, 8 parts of magnesium titanate powder, 6 parts of silicon micropowder and 10 parts of titanium dioxide powder.
The preparation process of the high dielectric alloy composite film for high frequency communication in example 1 is as follows:
(S1) preparing a high dielectric blending agent:
(S11) primary drying: respectively placing barium strontium titanate powder, calcium copper titanate powder, zinc zirconate powder, bismuth titanate powder, iron titanate powder, aluminum zirconate powder, magnesium titanate powder, silicon micropowder and titanium dioxide powder in an electric heating oven, and continuously drying for 24 hours at 200 ℃;
(S12) primary grinding: grinding the materials subjected to primary drying respectively by using a planetary ball mill, wherein hard alloy balls are adopted as grinding balls; the rotating speed of the ball mill is 400rpm; the diameter of the grinding ball is 5mm, 10mm and 15mm; ball material ratio: 20, a first step of; grinding time: 50h;
(S13) primary sieving: sieving the materials after primary grinding treatment by using an electric powder sieving machine respectively, wherein a sieve mesh is 325 meshes;
(S14) three-dimensional mixing: adding the materials after primary sieving into three-dimensional mixing equipment according to the preset proportion, wherein the rotating speed of a main shaft of the three-dimensional mixing equipment is 15rpm, and the time is 6 hours;
(S15) high-speed mixing: placing the three-dimensionally mixed materials in a high-speed mixing device, wherein the rotating speed of a stirring paddle of the high-speed mixing device is 1440rpm, and the time is 0.5h;
(S16) primary sintering: placing the high-speed mixed material in a high-temperature sintering furnace, and continuously sintering for 48 hours at 1150 ℃;
(S17) secondary grinding: grinding the primary sintered product by a planetary ball mill, wherein the grinding ball is a hard alloy ball; the rotating speed of the motor is as follows: 400rpm; grinding ball diameter: 5mm, 10mm, 15mm; ball material ratio: 2; grinding time: 50h;
(S18) secondary drying: continuously drying the materials subjected to secondary grinding for 48 hours at 200 ℃ by using an electric heating oven;
(S19) secondary sieving: sieving the material subjected to secondary drying by using an electric powder sieving machine, wherein a sieve mesh is 300 meshes;
(S2) preparing a polytetrafluoroethylene-based high-dielectric alloy composite film:
(S21) low-temperature high-speed mixing: adding polytetrafluoroethylene resin and a high dielectric blending agent into mixing equipment with a cooling device according to the adding proportion, wherein the adding proportion of the high dielectric blending agent is 29%, adding the polytetrafluoroethylene resin according to the rest proportion, and selecting the polytetrafluoroethylene resin prepared by a suspension method, wherein the embodiment adopts DF18A suspension resin (with the particle size of 30-40 microns) of Shandong Dongye polymer material Co., ltd.); during mixing, the temperature of the cooling liquid was 7 ℃:
(S211) firstly, controlling the rotating speed of the stirring paddle at 500rpm for 5min;
(S212) controlling the rotating speed of the stirring paddle at 900rpm for 3min;
(S213) standing for 5min;
(S214) repeating the steps (S211), (S212), and (S213) 3 times;
(S22) pressing: adding the powder after low-temperature high-speed mixing into a hydraulic press die, adopting an up-and-down bidirectional simultaneous pressurization mode, keeping the pressure for 2 hours after the plunger stops moving, slowly reducing the pressure to 0, and ejecting a composite film blank;
(S23) secondary sintering: placing the blank in a sintering furnace, closing a furnace door, slowly heating the sintering furnace from room temperature to 400 ℃, preserving heat for 20 hours, slowly reducing the temperature to room temperature, and taking out the composite film blank;
(S24) rotary cutting: fixing the composite film blank after secondary sintering on a mandrel, and enabling a turning tool to be parallel to the axis of the composite film blank to perform linear feeding motion;
(S25) slitting: and cutting the rotary-cut composite film blank into preset widths to obtain the polytetrafluoroethylene-based high-dielectric alloy composite film product.
The polytetrafluoroethylene-based high-dielectric alloy composite film for high-frequency communication prepared by the process has the dielectric constant of 2.95 and the dielectric loss of 0.012 at 10 GHz.
Example 2:
the high dielectric alloy composite film for high frequency communication in example 2 is prepared from 17% of a high dielectric blending agent and the balance of raw materials of polytetrafluoroethylene suspension resin, wherein the high dielectric blending agent is composed of the following raw materials in parts by mass: 45 parts of strontium barium titanate powder, 12 parts of copper calcium titanate powder, 4.5 parts of zinc zirconate powder, 1.8 parts of bismuth titanate powder, 0.4 part of iron titanate powder, 0.8 part of aluminum zirconate powder, 10 parts of magnesium titanate powder, 9 parts of silicon micropowder and 14 parts of titanium dioxide powder.
The preparation process of the high dielectric alloy composite film for high frequency communication in example 2 is as follows:
(T1) preparing a high dielectric blending agent:
(T11) primary drying: respectively placing strontium barium titanate powder, copper calcium titanate powder, zinc zirconate powder, bismuth titanate powder, iron titanate powder, aluminum zirconate powder, magnesium titanate powder, silicon micropowder and titanium dioxide powder in an electric heating oven, and continuously drying for 36 hours at 200 ℃;
(T12) primary grinding: grinding the materials after primary drying by adopting a planetary ball mill respectively, wherein hard alloy balls are adopted as grinding balls; the rotating speed of the ball mill is 300rpm; the diameter of the grinding ball is 5mm, 10mm and 15mm; ball material ratio: 10, a step of; grinding time: 27h;
(T13) one-pass sieving: sieving the materials subjected to primary grinding treatment by using an electric powder sieving machine respectively, wherein a sieve mesh is 250 meshes;
(T14) three-dimensional mixing: adding the materials after primary screening into three-dimensional mixing equipment according to the preset proportion, wherein the rotating speed of a main shaft of the three-dimensional mixing equipment is 12rpm, and the time is 4 hours;
(T15) high-speed mixing: placing the three-dimensionally mixed material in high-speed mixing equipment, wherein the rotating speed of a stirring paddle of the high-speed mixing equipment is 1170rpm, and the time is 2h;
(T16) primary sintering: placing the materials after high-speed mixing in a high-temperature sintering furnace, and continuously sintering for 60 hours at 800 ℃;
(T17) secondary grinding: grinding the primary sintered product by a planetary ball mill, wherein the grinding ball is a hard alloy ball; the rotating speed of the motor is as follows: 300rpm; grinding ball diameter: 5mm, 10mm, 15mm; ball material ratio: 10; grinding time: 25h;
(T18) Secondary drying: continuously drying the materials subjected to secondary grinding for 36 hours at 200 ℃ by using an electric heating oven;
(T19) double sieving: sieving the secondarily dried material by using an electric powder sieving machine, and sieving the sieved material by using a 320-mesh sieve;
(T2) preparation of a polytetrafluoroethylene-based high-dielectric alloy composite film:
(T21) low-temperature high-speed mixing: adding polytetrafluoroethylene resin and a high dielectric blending agent into mixing equipment with a cooling device according to the adding proportion, wherein the adding proportion of the high dielectric blending agent is 17%, adding the polytetrafluoroethylene resin according to the rest proportion, and selecting the polytetrafluoroethylene resin prepared by a suspension method, wherein the embodiment adopts DF18A suspension resin (with the particle size of 30-40 microns) of Shandong Dongye polymer material Co., ltd.); during mixing, the temperature of the cooling liquid is 5 ℃:
(T211) firstly, controlling the rotating speed of the stirring paddle at 600rpm for 10min;
(T212) controlling the rotating speed of the stirring paddle at 1000rpm for 5min;
(T213) standing for 30min;
(T214) repeating the steps (T211), (T212), and (T213) 3 times;
(T22) pressing: adding the powder after low-temperature high-speed mixing into a hydraulic press die, adopting an up-and-down bidirectional simultaneous pressurization mode, keeping the pressure for 2 hours after the plunger stops moving, slowly reducing the pressure to 0, and ejecting a composite film blank;
(T23) secondary sintering: placing the blank in a sintering furnace, closing a furnace door, slowly heating the sintering furnace from room temperature to 370 ℃, preserving heat for 20 hours, slowly reducing the temperature to room temperature, and taking out the composite film blank;
(T24) rotary cutting: fixing the composite film blank after secondary sintering on a mandrel, wherein a turning tool is parallel to the axis of the composite film blank and performs linear feeding motion;
(T25) slitting: and cutting the rotary-cut composite film blank into preset widths to obtain the polytetrafluoroethylene-based high-dielectric alloy composite film product.
The polytetrafluoroethylene-based high-dielectric alloy composite film for high-frequency communication prepared by the process has the dielectric constant of 3.01 and the dielectric loss of 0.014 at 10 GHz.
Example 3:
the high dielectric alloy composite film for high frequency communication in example 3 is prepared from 5% of a high dielectric blending agent and the balance of raw materials of polytetrafluoroethylene suspension resin, wherein the high dielectric blending agent is composed of the following raw materials in parts by mass: 60 parts of strontium barium titanate powder, 17 parts of copper calcium titanate powder, 6 parts of zinc zirconate powder, 2.9 parts of bismuth titanate powder, 0.6 part of iron titanate powder, 1.2 parts of aluminum zirconate powder, 12 parts of magnesium titanate powder, 12 parts of silicon micropowder and 18 parts of titanium dioxide powder.
The preparation process of the high dielectric alloy composite film for high frequency communication in example 3 is as follows:
(R1) preparation of high dielectric blending agent:
(R11) primary drying: respectively placing barium strontium titanate powder, calcium copper titanate powder, zinc zirconate powder, bismuth titanate powder, iron titanate powder, aluminum zirconate powder, magnesium titanate powder, silicon micropowder and titanium dioxide powder in an electric heating oven, and continuously drying for 48 hours at 200 ℃;
(R12) primary grinding: grinding the materials after primary drying by adopting a planetary ball mill respectively, wherein hard alloy balls are adopted as grinding balls; the rotating speed of the ball mill is 200rpm; the diameter of the grinding ball is 5mm, 10mm and 15mm; ball material ratio: 20, 1; grinding time: 5h;
(R13) one-pass sieving: sieving the materials subjected to primary grinding treatment by using an electric powder sieving machine respectively, wherein a sieve mesh is 180 meshes;
(R14) three-dimensional mixing: adding the materials after primary sieving into three-dimensional mixing equipment according to the preset proportion, wherein the rotating speed of a main shaft of the three-dimensional mixing equipment is 10rpm, and the time is 1h;
(R15) high speed mixing: placing the three-dimensionally mixed material in a high-speed mixing device, wherein the rotating speed of a stirring paddle of the high-speed mixing device is 900rpm, and the time is 4 hours;
(R16) primary sintering: placing the materials after high-speed mixing in a high-temperature sintering furnace, and continuously sintering for 72 hours at the temperature of 450 ℃;
(R17) Secondary grinding: grinding the primary sintering product by adopting a planetary ball mill, wherein a hard alloy ball is adopted as a grinding ball; the rotating speed of the motor is as follows: 200rpm; grinding ball diameter: 5mm, 10mm, 15mm; ball material ratio: 2; grinding time: 5h;
(R18) Secondary drying: continuously drying the materials subjected to secondary grinding for 24 hours at 200 ℃ by using an electric heating oven;
(R19) double sieving: sieving the secondarily dried material by using an electric powder sieving machine, wherein a sieve mesh is 350 meshes;
(R2) preparation of the polytetrafluoroethylene-based high-dielectric alloy composite film:
(R21) low temperature high speed mixing: adding polytetrafluoroethylene resin and a high dielectric blending agent into mixing equipment with a cooling device according to the adding proportion, wherein the adding proportion of the high dielectric blending agent is 5%, adding the polytetrafluoroethylene resin according to the rest proportion, and selecting the polytetrafluoroethylene resin prepared by a suspension method, wherein the embodiment adopts DF18A suspension resin (with the particle size of 30-40 microns) of Shandong Dongye polymer material Co., ltd.); during mixing, the temperature of the cooling liquid was 2 ℃:
(R211) firstly, controlling the rotating speed of the stirring paddle at 700rpm for 15min;
(R212) controlling the rotating speed of the stirring paddle at 1100rpm for 10min;
(R213) standing for 60min;
(R214) repeating steps (R211), (R212), and (R213) 3 times;
(R22) pressing: adding the powder after low-temperature high-speed mixing into a hydraulic press die, adopting an up-down bidirectional simultaneous pressurization mode, keeping the pressure for 2 hours after a plunger stops moving, slowly reducing the pressure to 0, and ejecting a composite film blank;
(R23) Secondary sintering: placing the blank in a sintering furnace, closing a furnace door, slowly heating the sintering furnace from room temperature to 350 ℃, preserving heat for 20 hours, slowly reducing the temperature to room temperature, and taking out the composite film blank;
(R24) rotary cutting: fixing the composite film blank after secondary sintering on a mandrel, and enabling a turning tool to be parallel to the axis of the composite film blank to perform linear feeding motion;
(R25) slitting: and cutting the rotary-cut composite film blank into preset widths to obtain the polytetrafluoroethylene-based high-dielectric alloy composite film product.
The polytetrafluoroethylene-based high-dielectric alloy composite film for high-frequency communication prepared by the process has the dielectric constant of 2.94 and the dielectric loss of 0.009 at 10 GHz.
All possible combinations of the technical features of the above embodiments may not be described for the sake of brevity, but should be considered as within the scope of the present disclosure as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that various changes and modifications can be made by those skilled in the art without departing from the spirit of the invention, and these changes and modifications are all within the scope of the invention. Therefore, the protection scope of the present patent should be subject to the appended claims.
Claims (7)
1. The high-dielectric alloy composite film for high-frequency communication is characterized by being prepared from a high-dielectric blending agent and polytetrafluoroethylene suspension resin, wherein the high-dielectric blending agent is prepared from the following raw materials in parts by weight: 30-60 parts of strontium barium titanate powder, 7-17 parts of copper calcium titanate powder, 3-6 parts of zinc zirconate powder, 0.7-2.9 parts of bismuth titanate powder, 0.2-0.6 part of iron titanate powder, 0.5-1.2 parts of aluminum zirconate powder, 8-12 parts of magnesium titanate powder, 6-12 parts of silicon micropowder and 10-18 parts of titanium dioxide powder.
2. The high-dielectric alloy composite film for high-frequency communication according to claim 1, wherein the high-dielectric blending agent comprises the following raw materials in parts by mass: 30 parts of strontium barium titanate powder, 7 parts of copper calcium titanate powder, 3 parts of zinc zirconate powder, 0.7 part of bismuth titanate powder, 0.2 part of iron titanate powder, 0.5 part of aluminum zirconate powder, 8 parts of magnesium titanate powder, 6 parts of silicon micropowder and 10 parts of titanium dioxide powder.
3. The high-dielectric alloy composite film for high-frequency communication according to claim 1, wherein the high-dielectric blending agent comprises the following raw materials in parts by mass: 45 parts of strontium barium titanate powder, 12 parts of copper calcium titanate powder, 4.5 parts of zinc zirconate powder, 1.8 parts of bismuth titanate powder, 0.4 part of iron titanate powder, 0.8 part of aluminum zirconate powder, 10 parts of magnesium titanate powder, 9 parts of silicon micropowder and 14 parts of titanium dioxide powder.
4. The high-dielectric alloy composite film for high-frequency communication according to claim 1, wherein the high-dielectric blending agent comprises the following raw materials in parts by mass: 60 parts of strontium barium titanate powder, 17 parts of copper calcium titanate powder, 6 parts of zinc zirconate powder, 2.9 parts of bismuth titanate powder, 0.6 part of iron titanate powder, 1.2 parts of aluminum zirconate powder, 12 parts of magnesium titanate powder, 12 parts of silicon micropowder and 18 parts of titanium dioxide powder.
5. A method for preparing a high dielectric alloy composite film for high frequency communication according to any one of claims 1 to 4, comprising the steps of:
(1) Preparing a high-dielectric blending agent:
(11) Primary drying: respectively placing barium strontium titanate powder, calcium copper titanate powder, zinc zirconate powder, bismuth titanate powder, iron titanate powder, aluminum zirconate powder, magnesium titanate powder, silicon micropowder and titanium dioxide powder in an electric heating oven, and continuously drying for 24-48h at 200 ℃;
(12) Primary grinding: grinding the materials after primary drying by adopting a planetary ball mill respectively, wherein hard alloy balls are adopted as grinding balls; the rotating speed of the ball mill is 200-400rpm; the diameter of the grinding ball is 5-15mm; ball material ratio: 2; grinding time: 5-50h;
(13) Primary sieving: sieving the materials after primary grinding by using an electric powder sieving machine respectively, wherein a sieve mesh is 180-325 meshes;
(14) Three-dimensional mixing: adding the materials after primary screening into three-dimensional mixing equipment according to a preset proportion, wherein the rotating speed of a main shaft of the three-dimensional mixing equipment is 10-15rpm, and the time is 1-6h;
(15) High-speed mixing: placing the three-dimensionally mixed materials in high-speed mixing equipment, wherein the rotating speed of a stirring paddle of the high-speed mixing equipment is 900-1440rpm, and the time is 0.5-4h;
(16) Primary sintering: placing the high-speed mixed material in a high-temperature sintering furnace, and continuously sintering for 48-72h at 450-1150 ℃;
(17) And (3) secondary grinding: grinding the primary sintered product by a planetary ball mill, wherein the grinding ball is a hard alloy ball; the rotating speed of the motor is as follows: 200-400rpm; grinding ball diameter: 5-15mm; ball material ratio: 2; grinding time: 5-50h;
(18) Secondary drying: continuously drying the materials subjected to secondary grinding for 24-48h at 200 ℃ by using an electric heating oven;
(19) And (3) secondary sieving: sieving the secondarily dried material by using an electric powder sieving machine, wherein a sieve mesh is 300-350 meshes;
(2) Preparing a polytetrafluoroethylene-based high-dielectric alloy composite film:
(21) Low-temperature high-speed mixing: adding polytetrafluoroethylene resin and a high dielectric blending agent into mixing equipment with a cooling device according to the addition proportion, wherein the addition proportion of the high dielectric blending agent is 5-29%, and the rest proportion is added with the polytetrafluoroethylene resin; during mixing, the temperature of the cooling liquid is 2-7 ℃, and the rotating speed of a stirring paddle is 500-1100rpm;
(22) Pressing: adding the powder after low-temperature high-speed mixing into a hydraulic press die, adopting an up-down bidirectional simultaneous pressurization mode, keeping the pressure at 50-260MPa and the pressing speed at 3-15mm/min, keeping the pressure for at least 2h after a plunger stops moving, slowly reducing the pressure to 0, and ejecting a composite film blank;
(23) And (3) secondary sintering: placing the blank in a sintering furnace, closing a furnace door, slowly heating the sintering furnace from room temperature to 350-400 ℃, keeping the temperature for at least 20h, slowly cooling the temperature to room temperature, and taking out the composite film blank;
(24) Rotary cutting: fixing the composite film blank after secondary sintering on a mandrel, wherein a turning tool is parallel to the axis of the composite film blank and performs linear feeding motion;
(25) Slitting: and cutting the rotary-cut composite film blank into preset widths to obtain the polytetrafluoroethylene-based high-dielectric alloy composite film product.
6. The method for preparing a high dielectric alloy composite film for high frequency communication according to claim 5, wherein the step (21) comprises:
(211) Firstly, controlling the rotating speed of a stirring paddle at 500-700rpm for 5-15min;
(212) Then the rotating speed of the stirring paddle is controlled to be 900-1100rpm, and the time is 3-10min;
(213) Standing for 5-60min;
(214) Repeating the steps (211), (212) and (213) 3-8 times.
7. The method for preparing a high dielectric alloy composite film for high frequency communication according to claim 5, wherein in the step (21), polytetrafluoroethylene resin prepared by a suspension method is selected, and the particle size of the resin is 15-150 μm.
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