CN110734614A - PTFE (Polytetrafluoroethylene) substrate material for high-frequency copper-clad plate and preparation method thereof - Google Patents
PTFE (Polytetrafluoroethylene) substrate material for high-frequency copper-clad plate and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
- C04B26/04—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B26/08—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing halogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/03—Use of materials for the substrate
- H05K1/0306—Inorganic insulating substrates, e.g. ceramic, glass
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/03—Use of materials for the substrate
- H05K1/0313—Organic insulating material
- H05K1/0353—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement
- H05K1/0373—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement containing additives, e.g. fillers
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00844—Uses not provided for elsewhere in C04B2111/00 for electronic applications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
Abstract
The invention relates to the field of material science and engineering, and aims to provide PTFE substrate materials for high-frequency copper-clad plates and a preparation method thereof, wherein the substrate materials consist of 100-x% of polytetrafluoroethylene and x% of modified ceramic powder in volume percentage, wherein x is more than or equal to 20 and less than or equal to 60, and the chemical formula of the modified ceramic powder is aBa (Co is aBa)1/3Nb2/3)O3‑(1‑a)Ba(Zn1/3Nb2/3)O3Wherein a is more than or equal to 0.2 and less than or equal to 0.7. The substrate material provided by the invention has high dielectric constant, low dielectric loss, proper dielectric constant temperature coefficient and proper resonant frequency temperatureA degree coefficient; meanwhile, the material has low thermal expansion coefficient, low water absorption and proper thermal conductivity. The preparation method disclosed by the invention is simple to operate, does not need special equipment and a complicated experimental process, is strong in universality, and has a good industrial basis and an application prospect.
Description
Technical Field
The invention relates to polytetrafluoroethylene substrate materials applied to a high-frequency copper-clad plate and a preparation method thereof, belonging to the field of material science and engineering.
Background
In recent years, with the development of 5G communication technology, satellite communication, radar system, automobile collision avoidance system, electronic navigation, and highly integrated circuit technology, electronic products are being developed to increase the frequency and speed of signal transmission. Printed Circuit Boards (PCBs) are important components of electronic devices, and play a great role in carrying, fixing components, circuit connection, signal transmission, and heat conduction. In order to ensure high-frequency and high-speed data transmission, the development of high-performance circuit substrates is important. At present, polymer-based composite substrate materials are increasingly becoming the current research hotspot due to the characteristics of simple preparation process, excellent comprehensive performance and the like. For high frequency circuit substrates, low dielectric constant and low dielectric loss are critical to ensure high speed signal transmission and integrity. The polytetrafluoroethylene has ultralow dielectric constant and dielectric loss, and is a polymer matrix material with great potential for being applied to high-performance circuits.
In order to ensure the practical application of the circuit substrate, the high-frequency substrate material has the comprehensive properties of temperature stability, thermal expansion coefficient matched with copper foil, low water absorption rate, high thermal conductivity and the like while meeting the requirements of proper dielectric constant and low dielectric loss. However, Polytetrafluoroethylene (PTFE) has the problems of large thermal expansion coefficient (109 ppm/DEG C), low thermal conductivity, poor dielectric constant and temperature stability and the like, so that the application expansion is limited, and modification is needed to meet the actual use requirement.
At present, the preparation of composite materials by filling PTFE with inorganic fillers such as ceramic, glass fiber and the like becomes the most common modification method and obtains definite effect, most of research focuses on the development and application of low dielectric constant substrate materials, but in recent years, the importance of developing high dielectric constant substrates is increasingly highlighted due to the special application requirement of high dielectric constantr＝6.7,tanδ＝0.003),BNT/PTFE(εr10.56, tan δ 0.004) and TeO2/PTFE(εrThe system of 5.4 and tan delta 0.006 has a significant disadvantage of higher dielectric loss ≧ 0.003, and recently newly published LMT/PTFE (. epsilon.) (r＝6.17,tanδ＝0.0019,τε＝123ppm/℃) And NLNT/PTFE (. epsilon.)r＝10.4,tanδ＝0.0026,τε0.9ppm/° c), the substrate material had excellent dielectric properties, but its water absorption rate (c:)>0.1%) is large and the importance of the coefficient of thermal expansion is neglected. Therefore, it is of great significance to develop a high dielectric constant substrate material having excellent overall properties.
Disclosure of Invention
The invention aims to solve the problem that the defects in the prior art are overcome, and PTFE substrate materials for high-frequency copper-clad plates and a preparation method thereof are provided.
In order to solve the technical problem, the solution of the invention is as follows:
substrate materials for high-frequency copper-clad plates are provided, the substrate materials consist of polytetrafluoroethylene accounting for 100-x% of the volume and modified ceramic powder of x%, wherein x is more than or equal to 20 and less than or equal to 60, and the chemical formula of the modified ceramic powder is aBa (Co is aBa)1/ 3Nb2/3)O3-(1-a)Ba(Zn1/3Nb2/3)O3Wherein a is more than or equal to 0.2 and less than or equal to 0.7.
The invention further provides a method for preparing the substrate material, which comprises the following steps:
(1) according to the molar ratio of 3: a to (1-a) to 2, taking powdery raw material BaCO3CoO, ZnO and Nb2O5A is more than or equal to 0.2 and less than or equal to 0.7, sintering for 4 hours at 1200 ℃ after ball milling is uniform, and grinding the sintered product in steps to obtain powdery ceramic filler;
(2) taking ceramic filler and coupling agent according to the mass ratio of 50: 1; dispersing the ceramic filler in ethanol, wherein the mass ratio of the ethanol to the ceramic filler is 6: 1; adding a coupling agent, stirring for 4 hours at 60 ℃, and drying at 120 ℃ to obtain the coupling agent modified ceramic filler;
(3) adding a coupling agent modified ceramic filler into PTFE emulsion according to the volume ratio of the components of the substrate material, namely (100-x)% PTFE and x% modified ceramic powder, wherein x is more than or equal to 20 and less than or equal to 60; stirring and dispersing uniformly to obtain a mixed dispersion liquid;
(4) adding ethanol into the mixed dispersion liquid, and stirring for 4 hours, wherein the addition amount of the ethanol is 15% of the mass of the mixed dispersion liquid; standing, filtering, and oven drying at 120 deg.C for 4 hr; removing the surfactant in the emulsion through heat treatment to obtain a mixture of PTFE and the modified filler;
(5) and crushing the mixture of PTFE and the modified filler into powder by using a ball mill, and carrying out hot-pressing sintering to obtain the substrate material for the high-frequency copper-clad plate.
In the invention, the ball milling time in the step (1) is 24 hours, and the granularity of the ceramic filler after ball milling is 0.2-1 μm.
In the invention, the coupling agent in the step (2) is KH550, F8261 or Z6124; the density of the coupling agent was 1.34g/cm3The mass fraction is 97%.
In the present invention, the PTFE emulsion in the step (3) has a mass concentration of 1.51g/cm3The solid content was 60%.
In the invention, the temperature of the heat treatment in the step (4) is 280 ℃ and the time is 4 hours.
In the invention, the rotation speed of the ball mill is controlled to be 300r/min when the ball mill is used for crushing in the step (5), and the particle size of the powder after ball milling is 200-400 mu m.
In the invention, when hot-pressing sintering is carried out in the step (5), the hot-pressing pressure is controlled to be 25MPa, the hot-pressing time is 2 hours, and the hot-pressing temperature is 360-380 ℃.
Description of the inventive principles:
the modified ceramic powder used in the present invention has a chemical formula of aBa (Co)1/3Nb2/3)O3-(1-a)Ba(Zn1/3Nb2/3)O3Wherein a is more than or equal to 0.2 and less than or equal to 0.7. Unlike the prior art, which also commonly uses ceramic-filled PTFE to prepare composites, the ceramic powder used in the present invention has a high dielectric constant (ε) compared to conventional ceramic powdersr33.5), high Q × f (Q × f 80000GHz) and stable temperature coefficient of resonance frequency (τ)f4.2 ppm/DEG C), can improve the dielectric constant of the composite material, keep the lower dielectric loss of the composite material and improve the dielectric constant of the composite material after being applied to the composite materialTemperature coefficient, which is not realized by common ceramic powder. Since those skilled in the art will typically focus research and development efforts on the development of low-k substrate materials, progress has not always been achieved in high-k substrate materials with suitable overall properties.
Because PTFE is difficult to process relative to other organic matters, in the prior art, when the ceramic powder filled PTFE composite substrate material is prepared, the processes of mixing, blank making, extruding, calendering, drying and hot pressing are required, and equipment such as an extruder and a calender are required. Due to the improvement of the preparation process, the method does not need special equipment and a complicated experimental process, and has strong universality.
Compared with the prior art, the invention has the beneficial effects that:
1. the substrate material provided by the invention has excellent dielectric properties: high dielectric constant (>6) Low dielectric loss (tan delta is less than or equal to 0.003), proper temperature coefficient of dielectric constant (-334.7 ppm/DEG C to-75.2 ppm/DEG C), proper temperature coefficient of resonance frequency (10.7 ppm/DEG C to 79.9 ppm/DEG C); simultaneously has low thermal expansion coefficient (26.9 ppm/DEG C-87.5 ppm/DEG C), low water absorption (0.024-1.66 percent) and proper thermal conductivity (0.39 W.m)-1·K-1～0.48W·m-1·K-1)。
2. The method is simple to operate, does not need special equipment and a complicated experimental process, has strong universality, and has good industrialization foundation and application prospect.
3. The high-frequency copper-clad plate prepared by the substrate material can bring the technical effects of high dielectric constant, low dielectric loss, stable temperature coefficient, low water absorption, proper thermal expansion coefficient and thermal conductivity in step .
Detailed Description
The present invention will be further described in with reference to the following examples, which are not intended to limit the scope of the present invention.
The method for preparing the substrate material for the high-frequency copper-clad plate comprises the following steps:
(1) taking the powder according to the molar ratio of 3: a to (1-a) to 2Powdery raw material BaCO3CoO, ZnO and Nb2O5A is more than or equal to 0.2 and less than or equal to 0.7, ball milling is carried out for 24 hours, then sintering is carried out for 4 hours at 1200 ℃, and -step grinding is carried out until the granularity is 0.2-1 mu m, thus obtaining the ceramic filler;
(2) taking ceramic filler and coupling agent according to the mass ratio of 50: 1, dispersing the ceramic filler in ethanol, controlling the mass ratio of the ethanol to the ceramic filler to be 6: 1, adding the coupling agent, stirring for 4 hours at 60 ℃, and drying at 120 ℃ to obtain the coupling agent modified ceramic filler, wherein the coupling agent is any of KH550, F8261 and Z6124, and the mass concentration of the coupling agent is 1.33g/cm3The mass fraction is 97 percent;
(3) adding a coupling agent modified ceramic filler into PTFE emulsion according to the composition (100-x) vol% of PTFE and x vol% of modified ceramic powder (wherein x is more than or equal to 20 and less than or equal to 60) of the substrate material, and uniformly stirring and dispersing to obtain a mixed dispersion liquid; the mass concentration of the PTFE emulsion is 1.51g/cm3The mass fraction is 60 percent;
(4) adding ethanol into the mixed dispersion liquid, wherein the addition amount of the ethanol is 15% of the mass of the mixed dispersion liquid; continuously stirring for 4h, standing, filtering, drying at 120 ℃ for 4h, and performing heat treatment at 280 ℃ for 4h to remove the surfactant in the emulsion to obtain a mixture of PTFE and the modified filler;
(5) and crushing the mixture of PTFE and the modified filler into powder by using a ball mill, and then preparing the substrate material for the high-frequency copper-clad plate by hot-pressing sintering. In the step, the rotating speed of the ball mill is controlled to be 300r/min, and the particle size of the powder after ball milling is 200-400 microns. The hot pressing pressure is 25MPa, and the hot pressing time is 2 h; the hot pressing temperature is 360-380 ℃.
The substrate material finally prepared consists of (100-x) vol% (volume percentage) of polytetrafluoroethylene and xvol% of ceramic powder, wherein x is more than or equal to 20 and less than or equal to 60; the chemical formula of the ceramic powder is aBa (Co)1/3Nb2/3)O3-(1-a)Ba(Zn1/3Nb2/3)O3Wherein a is more than or equal to 0.2 and less than or equal to 0.7.
Table 1 shows the recipe compositions and the preparation process parameters in the examples
The properties of the products obtained in the examples were examined with reference to the test method published by IPC-TM-650, and the data shown in Table 2 were obtained.
Table 2 shows the properties of the products obtained in the examples
From the data of the above examples, it can be seen that when a is 0.7 and the volume fraction of the ceramic powder is 50%, the PTFE composite substrate material has a high dielectric constant of 7.7, a low dielectric loss of 0.0014, a suitable temperature coefficient of dielectric constant of-125.6 ppm/° c and a temperature coefficient of resonant frequency of 29.5ppm/° c, a low water absorption of 0.07%, a low thermal expansion coefficient of 33.3ppm/° c, and a suitable thermal conductivity of 0.46W · m-1·K-1And the like, and is suitable for high-frequency copper clad laminates.
An example of the application method of the substrate material is as follows:
the substrate material is combined and laminated with a prepreg, copper foil and the like, and a high-frequency copper-clad plate can be obtained after hot pressing, and can be applied to radar systems, communication systems, navigation systems and high-integration circuits.
Claims (8)
1, base plate material for high-frequency copper-clad plate, which is characterized in that the base plate material is composed of 100-x% of polytetrafluoroethylene and x% of modified ceramic powder, wherein x is more than or equal to 20 and less than or equal to 60, and the chemical formula of the modified ceramic powder is aBa (Co is aBa)1/3Nb2/3)O3-(1-a)Ba(Zn1/3Nb2/3)O3Wherein a is more than or equal to 0.2 and less than or equal to 0.7.
2. A method of preparing a substrate material according to claim 1, comprising the steps of:
(1) according to the molar ratio of 3: a to (1-a) to 2, taking powdery raw material BaCO3CoO, ZnO and Nb2O5A is more than or equal to 0.2 and less than or equal to 0.7, sintering for 4 hours at 1200 ℃ after ball milling is uniform, and grinding the sintered product in steps to obtain powdery ceramic filler;
(2) taking ceramic filler and coupling agent according to the mass ratio of 50: 1; dispersing the ceramic filler in ethanol, wherein the mass ratio of the ethanol to the ceramic filler is 6: 1; adding a coupling agent, stirring for 4 hours at 60 ℃, and drying at 120 ℃ to obtain the coupling agent modified ceramic filler;
(3) adding a coupling agent modified ceramic filler into PTFE emulsion according to the volume ratio of the components of the substrate material, namely (100-x)% PTFE and x% modified ceramic powder, wherein x is more than or equal to 20 and less than or equal to 60; stirring and dispersing uniformly to obtain a mixed dispersion liquid;
(4) adding ethanol into the mixed dispersion liquid, and stirring for 4 hours, wherein the addition amount of the ethanol is 15% of the mass of the mixed dispersion liquid; standing, filtering, and oven drying at 120 deg.C for 4 hr; removing the surfactant in the emulsion through heat treatment to obtain a mixture of PTFE and the modified filler;
(5) and crushing the mixture of PTFE and the modified filler into powder by using a ball mill, and carrying out hot-pressing sintering to obtain the substrate material for the high-frequency copper-clad plate.
3. The method of claim 2, wherein the ball milling time in the step (1) is 24 hours, and the particle size of the ceramic filler after ball milling is 0.2-1 μm.
4. The process according to claim 2, wherein the coupling agent in step (2) is KH550, F8261 or Z6124; the density of the coupling agent was 1.34g/cm3The mass fraction is 97%.
5. The method according to claim 2, wherein the PTFE emulsion in the step (3) has a mass concentration of 1.51g/cm3The solid content was 60%.
6. The method according to claim 2, wherein the temperature of the heat treatment in the step (4) is 280 ℃ and the time is 4 hours.
7. The method according to claim 2, wherein the rotation speed of the ball mill is controlled to be 300r/min during the crushing with the ball mill in the step (5), and the particle size of the powder after ball milling is 200-400 μm.
8. The method according to claim 2, wherein in the hot pressing sintering in the step (5), the hot pressing pressure is controlled to be 25MPa, the hot pressing time is 2 hours, and the hot pressing temperature is 360-380 ℃.
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| CN111642076A (en) * | 2020-04-29 | 2020-09-08 | 信维通信（江苏）有限公司 | Manufacturing process of two-dimensional material filled copper-clad plate |
| CN113061311A (en) * | 2021-04-21 | 2021-07-02 | 山东森荣新材料股份有限公司 | PTFE modified membrane for high-frequency copper-clad plate |
| CN113365426A (en) * | 2020-04-21 | 2021-09-07 | 广州市东泓氟塑料股份有限公司 | Novel high-frequency high-speed flexible copper-clad plate and preparation method and application thereof |
| CN114479191A (en) * | 2022-01-12 | 2022-05-13 | 山东国瓷功能材料股份有限公司 | Inorganic filler for PTFE (polytetrafluoroethylene) -based copper-clad plate and preparation method thereof |
| CN114527169A (en) * | 2022-01-28 | 2022-05-24 | 山东国瓷功能材料股份有限公司 | Method for testing dielectric property of ceramic material and application thereof |
| CN114989548A (en) * | 2022-06-30 | 2022-09-02 | 浙江华正新材料股份有限公司 | Glue solution, film and circuit board |
| CN115322500A (en) * | 2022-08-30 | 2022-11-11 | 哈尔滨工业大学（深圳） | Polytetrafluoroethylene prepreg, preparation method thereof and copper-clad plate |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113365426A (en) * | 2020-04-21 | 2021-09-07 | 广州市东泓氟塑料股份有限公司 | Novel high-frequency high-speed flexible copper-clad plate and preparation method and application thereof |
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| CN114479191A (en) * | 2022-01-12 | 2022-05-13 | 山东国瓷功能材料股份有限公司 | Inorganic filler for PTFE (polytetrafluoroethylene) -based copper-clad plate and preparation method thereof |
| CN114527169A (en) * | 2022-01-28 | 2022-05-24 | 山东国瓷功能材料股份有限公司 | Method for testing dielectric property of ceramic material and application thereof |
| CN114527169B (en) * | 2022-01-28 | 2024-02-02 | 山东国瓷功能材料股份有限公司 | Method for testing dielectric property of ceramic material and application thereof |
| CN114989548A (en) * | 2022-06-30 | 2022-09-02 | 浙江华正新材料股份有限公司 | Glue solution, film and circuit board |
| CN114989548B (en) * | 2022-06-30 | 2024-01-09 | 浙江华正新材料股份有限公司 | Glue solution, film and circuit substrate |
| CN115322500A (en) * | 2022-08-30 | 2022-11-11 | 哈尔滨工业大学（深圳） | Polytetrafluoroethylene prepreg, preparation method thereof and copper-clad plate |
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