CN104496268B - A kind of preparation method of high frequency high dielectric microwave composite medium substrate - Google Patents

A kind of preparation method of high frequency high dielectric microwave composite medium substrate Download PDF

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CN104496268B
CN104496268B CN201410774975.XA CN201410774975A CN104496268B CN 104496268 B CN104496268 B CN 104496268B CN 201410774975 A CN201410774975 A CN 201410774975A CN 104496268 B CN104496268 B CN 104496268B
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ceramics
temperature
medium substrate
high frequency
composite medium
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CN104496268A (en
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宋永要
张立欣
王丽婧
赵元成
徐永宽
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CETC 46 Research Institute
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Abstract

The preparation method that the present invention relates to a kind of high frequency high dielectric microwave composite medium substrate. Its step: first mixed with formic acid solution by ceramics in proportion, be subsequently adding a certain amount of silane coupler, adds resin, and heated and stirred, drying obtain pottery mixed powder; Being tiled in a mold by pottery mixed powder, concussion makes it smooth repeatedly; Mould after charging is put into cold moudling in hot press, and temperature is room temperature, and pressure is 3 ~ 12MPa; Finally the substrate two sides after cold moudling is covered with Copper Foil respectively, is placed again in mould, pressing sintering carries out hot pressed sintering, at temperature 350 ~ 390 DEG C, be incubated 2 ~ 10h, pressure 5 ~ 22Mpa, afterwards natural cooling. The high frequency high dielectric microwave composite medium substrate that employing a process for preparing has mechanical performance excellence, dielectric constant is high, dielectric loss is low, homogeneity good and consistency high, thus meeting the market demand to high frequency high dielectric microwave composite medium substrate.

Description

A kind of preparation method of high frequency high dielectric microwave composite medium substrate
Technical field
The present invention relates to microwave composite medium substrate to prepare, the preparation method particularly relating to a kind of high frequency high dielectric microwave composite medium substrate.
Background technology
Along with the high speed development of information industry, the demand of high-frequency microwave baseplate material is soared, and microelectric technique also fast development therewith, the demand of the miniature antenna can coordinated with instrument size and have effective electrical property is further urgent. Along with GPS acts on day by day notable in real life, RF front-end module tends to portable day by day: light, thin, short, little. Therefore, one of compact in size problem also Main Topics just having become microstrip antenna how solving antenna. The method that one of which is commonly used is exactly that the dielectric substrate adopting high-k is to reduce microstrip antenna size. Traditional printed circuit board industry is mainly based on infusion process, and by joining glue, gluing, the technique such as overlapping, pressing plate and sintering prepares copper-clad plate, but the composite base plate being filler with ceramics cannot adopt above-mentioned preparation technology.
Summary of the invention
In view of above-mentioned prior art situation, the preparation method that the present invention provides a kind of high frequency high dielectric microwave composite medium substrate. The method is a kind of novel preparation process, namely prepares high performance microwave composite base plate by stone+cold moudling+Thermocompressed sintering and forming method.
The present invention is realized by following processing step: the preparation method of a kind of high frequency high dielectric microwave composite medium substrate, it is characterised in that this preparation method comprises the steps:
(1). hybrid technique
(1). ceramics and formic acid solution are sufficiently mixed stirring 1h in proportion in homogenizer;
(2). adding silane coupler, heated and stirred 1 ~ 2h in (1) step mixed solution, temperature is 60 ~ 100 DEG C;
(3). in (2) step mixed solution, add resin, continue heated and stirred 3 ~ 5h;
(4). the mixed solution mechanical pump sucking filtration that (3) step is obtained, and rinse 3 ~ 5 times with alcoholic solution, at temperature 120 ~ 300 DEG C, then dry 3 ~ 30h, obtain pottery mixed powder;
Wherein: the weight of described ceramics accounts for the 45 ~ 65% of ceramics and total resin weight; Silane coupler accounts for the 1 ~ 2% of ceramics weight; Resin accounts for the 35 ~ 55% of ceramics and total resin weight; The weight ratio of ceramics and formic acid solution is 100:65; Described resin adopts one or both in politef and perfluoroethylene-propylene;
(2). stone technique
Being tiled in a mold by ceramic mixed powder after drying, concussion makes it smooth repeatedly;
(3). cooling formation technic
Mould after charging is put into cold moudling in hot press, and temperature is room temperature, and pressure is 3 ~ 12MPa;
(4). sintering process
Substrate two sides after cold moudling is covered with Copper Foil respectively, is placed again in mould, pressing sintering carries out hot pressed sintering, at temperature 350 ~ 390 DEG C, be incubated 2 ~ 10h, pressure 5 ~ 22Mpa, afterwards natural cooling.
The invention have the advantages that: the high frequency high dielectric microwave composite medium substrate that employing a process for preparing has mechanical performance excellence, dielectric constant is high, dielectric loss is low, homogeneity good and consistency high, thus meeting the market demand to high frequency high dielectric microwave composite medium substrate.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1:
(1) hybrid technique
It is that 45% ceramics is put in homogenizer with 30g formic acid solution by weight ratio, stirring mixing 1h, being subsequently added weight ratio is 1.5% silane coupler, heated and stirred 1h, and temperature is 90 DEG C; Adding weight ratio is 55% politef, continues heated and stirred 5h; The mixed solution mechanical pump sucking filtration that will obtain, and rinse 3 times with alcoholic solution, each 50ml, at temperature 280 DEG C, then dry 20h, obtain pottery mixed powder.
(2) stone technique
Weighing a certain amount of pottery mixed powder according to mould size and required sheet metal thickness, tiling in a mold, is repeatedly shaken with steel ruler and is made it smooth.
(3) cold pressing forming process
Mould after charging is put into cold moudling in hot press, and temperature is room temperature, and pressure is 7MPa.
(4) sintering process
Substrate two sides after molding is covered with Copper Foil respectively, is placed again in mould, pressing sintering carries out hot pressed sintering, at temperature 380 DEG C, be incubated 2h, pressure 20Mpa, afterwards natural cooling.
Embodiment 2:
(1) hybrid technique
It is that 55% ceramics is put in homogenizer with 36g formic acid solution by weight ratio, stirring mixing 1h, being subsequently added weight ratio is 1.5% silane coupler, heated and stirred 2h, and temperature is 90 DEG C; Adding weight ratio is 10% perfluoroethylene-propylene and 35% politef, continues heated and stirred 3h; The mixed solution mechanical pump sucking filtration that will obtain, and rinse 5 times with alcoholic solution, each 50ml, at temperature 260 DEG C, then dry 18h, obtain pottery mixed powder.
(2) stone technique
Weighing a certain amount of pottery mixed powder according to mould size and required sheet metal thickness, tiling in a mold, is repeatedly shaken with steel ruler and is made it smooth.
(3) cold pressing forming process
Mould after charging is put into cold moudling in hot press, and temperature is room temperature, and pressure is 5MPa.
(4) sintering process
Substrate two sides after molding is covered with Copper Foil respectively, is placed again in mould, pressing sintering carries out hot pressed sintering, at temperature 370 DEG C, be incubated 2h, pressure 17Mpa, afterwards natural cooling.
Embodiment 3:
(1) hybrid technique
It is that 65% ceramics is put in homogenizer with 43g formic acid solution by weight ratio, stirring mixing 1h, being subsequently added weight ratio is 1.5% silane coupler, heated and stirred 1h, and temperature is 70 DEG C; Adding weight ratio is 35% politef, continues heated and stirred 3h; The mixed solution mechanical pump sucking filtration that will obtain, and rinse 5 times with alcoholic solution, each 50ml, at temperature 280 DEG C, then dry 19h, obtain pottery mixed powder.
(2) stone technique
Weighing a certain amount of pottery mixed powder according to mould size and required sheet metal thickness, tiling in a mold, is repeatedly shaken with steel ruler and is made it smooth.
(3) cold pressing forming process
Mould after charging is put into cold moudling in hot press, and temperature is room temperature, and pressure is 10MPa.
(4) sintering process
Substrate two sides after molding is covered with Copper Foil respectively, is placed again in mould, pressing sintering carries out hot pressed sintering, at temperature 375 DEG C, be incubated 2h, pressure 22Mpa, afterwards natural cooling.
After testing, the high frequency high dielectric microwave composite medium substrate performance indications such as following table that prepared by three above embodiment:
Dielectric constant Dielectric loss
Embodiment 1 6.2 1.4��10-3
Embodiment 2 7.6 1.8��10-3
Embodiment 3 9.8 2.1��10-3
Embodiment 1: requiring that under 10GHz, dielectric constant reaches 4 ~ 7, dielectric loss is less than 2.4 �� 10-3;
Embodiment 2: requiring that under 10GHz, dielectric constant reaches 5 ~ 8, dielectric loss is less than 2.3 �� 10-3;
Embodiment 3: requiring that under 10GHz, dielectric constant reaches 9 ~ 11, dielectric loss is less than 2.7 �� 10-3��
The performance indications testing result of three above embodiment all meets the requirements.
The preparating mechanism of the present invention: first ceramics is hydrolyzed in formic acid solution, form alcoholic extract hydroxyl group, it is subsequently adding silane coupler, silane coupler one end after hydrolysis and alcoholic extract hydroxyl group react, the other end forms covalent bond with the fluorine atom in resin, make ceramics and resin-bonded tight, mix homogeneously.

Claims (1)

1. the preparation method of a high frequency high dielectric microwave composite medium substrate, it is characterised in that this preparation method comprises the steps:
(1). hybrid technique
(1). ceramics and formic acid solution are sufficiently mixed stirring 1h in proportion in homogenizer;
(2). adding silane coupler, heated and stirred 1 ~ 2h in (1) step mixed solution, temperature is 60 ~ 100 DEG C;
(3). in (2) step mixed solution, add resin, continue heated and stirred 3 ~ 5h;
The mixed solution mechanical pump sucking filtration that (3) step is obtained, and rinse 3 ~ 5 times with alcoholic solution, at temperature 120 ~ 300 DEG C, then dry 3 ~ 30h, obtain pottery mixed powder;
Wherein: the weight of described ceramics accounts for the 45 ~ 65% of ceramics and total resin weight; Silane coupler accounts for the 1 ~ 2% of ceramics weight; Resin accounts for the 35 ~ 55% of ceramics and total resin weight; The weight ratio of ceramics and formic acid solution is 100:65; Described resin adopts one or both in politef and perfluoroethylene-propylene;
(2). stone technique
Being tiled in a mold by ceramic mixed powder after drying, concussion makes it smooth repeatedly;
(3). cooling formation technic
Putting in hot press compressing by the mould after charging, temperature is room temperature, and pressure is 3 ~ 12MPa;
(4). sintering process
Substrate two sides after compressing is covered with Copper Foil respectively, is placed again in mould, pressing sintering carries out hot pressed sintering, at temperature 350 ~ 390 DEG C, be incubated 2 ~ 10h, pressure 5 ~ 22MPa, afterwards natural cooling.
CN201410774975.XA 2014-12-16 2014-12-16 A kind of preparation method of high frequency high dielectric microwave composite medium substrate Active CN104496268B (en)

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Publication number Priority date Publication date Assignee Title
CN105130423B (en) * 2015-07-15 2017-05-24 中国电子科技集团公司第四十六研究所 Preparation technology of microwave composite dielectric substrate based on barium titanate-type ceramic powder
CN106671517A (en) * 2016-07-06 2017-05-17 武汉联恒电子材料有限公司 Composition of fluorine-containing resin and compound ceramic fillers and high-frequency copper-clad laminate manufactured from composition
CN108329626B (en) * 2017-01-20 2020-10-27 江西安缔诺科技有限公司 Composite microwave dielectric material and manufacturing method thereof
CN108901130A (en) * 2018-05-18 2018-11-27 吴东建 A kind of high-frequency high-speed flexibility coat copper plate and preparation method thereof
CN109760384A (en) * 2018-12-24 2019-05-17 嘉兴佳利电子有限公司 A kind of preparation method of high dielectric constant composite laminate
CN111775527A (en) * 2020-07-09 2020-10-16 瑞声科技(南京)有限公司 Preparation method of composite medium copper-clad plate and printed circuit board
CN112757552B (en) * 2020-12-18 2023-03-24 南京锐码毫米波太赫兹技术研究院有限公司 Preparation method of dielectric substrate for millimeter wave terahertz frequency band
CN113211903A (en) * 2021-06-03 2021-08-06 中国振华集团云科电子有限公司 Production method of ceramic-filled type hydrocarbon resin copper-clad plate

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5693517A (en) * 1979-12-25 1981-07-29 Sumitomo Alum Smelt Co Ltd Forming method for composite film of ethylene tetrafluoride resin
CN1799830A (en) * 2005-12-30 2006-07-12 顾根山 Wide-dielectric constant polytetrafluoroethylene glass cloth coated copper foil plate
CN101564918A (en) * 2009-05-19 2009-10-28 顾根山 Metal-based composite medium copper-clad foil plate
CN103066186A (en) * 2013-01-07 2013-04-24 浙江华正新材料股份有限公司 Insulating layer and aluminum substrate of ceramic chip composite structure and manufacturing method of the same

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5693517A (en) * 1979-12-25 1981-07-29 Sumitomo Alum Smelt Co Ltd Forming method for composite film of ethylene tetrafluoride resin
CN1799830A (en) * 2005-12-30 2006-07-12 顾根山 Wide-dielectric constant polytetrafluoroethylene glass cloth coated copper foil plate
CN101564918A (en) * 2009-05-19 2009-10-28 顾根山 Metal-based composite medium copper-clad foil plate
CN103066186A (en) * 2013-01-07 2013-04-24 浙江华正新材料股份有限公司 Insulating layer and aluminum substrate of ceramic chip composite structure and manufacturing method of the same

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