WO2022247508A1 - 5g高频覆铜板用陶瓷改性ptfe薄膜的加工方法 - Google Patents

5g高频覆铜板用陶瓷改性ptfe薄膜的加工方法 Download PDF

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WO2022247508A1
WO2022247508A1 PCT/CN2022/086689 CN2022086689W WO2022247508A1 WO 2022247508 A1 WO2022247508 A1 WO 2022247508A1 CN 2022086689 W CN2022086689 W CN 2022086689W WO 2022247508 A1 WO2022247508 A1 WO 2022247508A1
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ceramic
blank
film
ceramic membrane
membrane blank
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PCT/CN2022/086689
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English (en)
French (fr)
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杨文光
孙克原
张敏华
余辉
徐小曼
王孝刚
徐辉
夏炎
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南京肯特复合材料股份有限公司
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Publication of WO2022247508A1 publication Critical patent/WO2022247508A1/zh

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
    • B29C43/006—Pressing and sintering powders, granules or fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B13/00—Conditioning or physical treatment of the material to be shaped
    • B29B13/02—Conditioning or physical treatment of the material to be shaped by heating
    • B29B13/021—Heat treatment of powders
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B13/00—Conditioning or physical treatment of the material to be shaped
    • B29B13/10—Conditioning or physical treatment of the material to be shaped by grinding, e.g. by triturating; by sieving; by filtering
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/02—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
    • B29B7/22—Component parts, details or accessories; Auxiliary operations
    • B29B7/28—Component parts, details or accessories; Auxiliary operations for measuring, controlling or regulating, e.g. viscosity control
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
    • B29C43/003—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor characterised by the choice of material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
    • B29C43/02—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
    • B29C43/32—Component parts, details or accessories; Auxiliary operations
    • B29C43/58—Measuring, controlling or regulating
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
    • B29C43/32—Component parts, details or accessories; Auxiliary operations
    • B29C43/58—Measuring, controlling or regulating
    • B29C2043/5808—Measuring, controlling or regulating pressure or compressing force
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • 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
    • C08J2327/12—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 containing fluorine atoms
    • C08J2327/18—Homopolymers or copolymers of tetrafluoroethylene
    • 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
    • C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
    • C08K3/013—Fillers, pigments or reinforcing additives

Definitions

  • the invention belongs to the technical field of high-frequency and ultra-high-frequency wireless communication, and specifically relates to a processing method of a ceramic modified PTFE film for a 5G high-frequency copper-clad laminate.
  • the ceramic-modified PTFE film can be used as a high-frequency copper-clad laminate and a multilayer high-speed laminate
  • the base material of copper plate is used.
  • the vertical sintering method is usually used during sintering. Due to the weight of the blank, the size difference between the upper and lower ends of the blank after sintering is too large (that is, the phenomenon of large and small ends), and the blank is deformed, resulting in the turning of the film. The material waste is large, which increases the cost.
  • the technical problem to be solved by this invention is to provide a kind of processing method of ceramic modified PTFE film for 5G high-frequency copper-clad laminate for above-mentioned deficiencies in the prior art, the processing method of this 5G high-frequency copper-clad laminate ceramic modified PTFE film can improve The uniformity of the ceramic powder dispersion, the uniformity of the film thickness and the uniformity of the film layer are good, and the processing difficulty is small, which can meet the needs of mass production and has high practicability.
  • a processing method for a ceramic modified PTFE film for a 5G high-frequency copper-clad laminate comprising the following steps:
  • step (1) is specifically:
  • the ceramic powder is subjected to high temperature heat treatment, the particle size of the ceramic powder is 1um-6um, the heat treatment temperature is 400°C-600°C, and the heat treatment time is 24h-72h.
  • step (2) is specifically:
  • Sieve the above-mentioned treated ceramic powder with a 200-mesh sieve, then roughly mix the polytetrafluoroethylene suspension resin, ceramic powder and high-temperature dispersant, and then use a mixer for fine mixing after rough mixing.
  • the sieve aperture is 0.5mm-1.0mm
  • the speed of the mixer is 1500r/min-3600r/min
  • the mixing frequency is 5-15 times.
  • the mass percentage of the polytetrafluoroethylene suspension resin is 65% to 95%, and the mass percentage of the ceramic powder is 4.5% to 30%.
  • the mass percent of the high-temperature dispersant is 0.5% to 5%.
  • step (3) is specifically:
  • the outer diameter of the ceramic membrane blank is 560mm-580mm, and the axial length is ⁇ 500mm.
  • step (4) is specifically:
  • the ceramic membrane blank is sintered horizontally in a sintering furnace. When the temperature is below 40°C, the ceramic membrane blank does not rotate. When the temperature is 40°C to 360°C, the rotation speed of the ceramic membrane blank is 1r/h to 3r/h. During the cooling process, The rotational speed of the ceramic membrane blank is 2r/h ⁇ 4r/h.
  • step (5) is specifically:
  • the present invention adopts the method of high heat treatment of ceramic powder to selectively remove surface coupling agent and other substances, retain some active groups, avoid ceramic powder agglomeration and poor dispersion during the mixing process; reduce the proportion of surface hydroxyl groups; improve high frequency Copper-clad laminate anti-CAF (conductive anode filament) capability; the PCB prepared by using the ceramic modified PTFE film of the present invention meets the tracking resistance CTI>600V.
  • the present invention adds a high-temperature dispersant in the preparation process, which improves the uniformity of ceramic powder dispersion.
  • the polytetrafluoroethylene suspension resin, ceramic powder and high-temperature dispersant are blended using a mixer.
  • the mixing method has good uniformity. It can be produced in batches, and the processing difficulty is small; the invention adopts the rotary cutting film technology, which can realize uniform film thickness, wide film, and high practicability; it can meet the actual high-frequency and ultra-high-frequency copper-clad laminate substrates with a width of more than 500mm Membrane use.
  • the ceramic membrane blank of the present invention adopts horizontal rotary sintering technology, that is, the axis of the cylindrical blank is in a horizontal state, and the axis of the cylindrical blank is used as the center line to rotate and sinter in the sintering furnace, which avoids the large and small ends that are easy to appear in standing sintering
  • the disadvantages are that the outer diameter of the blank after sintering is about 5mm higher and lower, and the material loss caused by turning the film is a normal loss.
  • a processing method for a ceramic modified PTFE film for a 5G high-frequency copper-clad laminate comprising the following steps:
  • Ceramic powder is subjected to high-temperature heat treatment, the particle diameter of described ceramic powder is D501um, heat treatment temperature is 400 °C, and heat treatment time is 72h;
  • the whole sintering process includes three stages of heating, heat preservation and cooling.
  • the heating stage and cooling stage need to be slow to ensure the uniformity of the ceramic blank temperature. It is enough to burn through the ceramic blank;
  • this embodiment adopts the horizontal rotary sintering technology of the cylindrical blank, that is, the ceramic membrane blank is sintered horizontally in the blast sintering furnace, and there is no rotation at 40°C, and the rotation speed is 1r at 40°C to 360°C /h, the speed is 2r/h during the cooling process;
  • a processing method for a ceramic modified PTFE film for a 5G high-frequency copper-clad laminate comprising the following steps:
  • Ceramic powder is subjected to high-temperature heat treatment, the particle diameter of described ceramic powder is D50 3um, heat treatment temperature is 500 °C, and heat treatment time is 48h;
  • the whole sintering process includes three stages of heating, heat preservation and cooling.
  • the heating stage and cooling stage need to be slow to ensure the uniformity of the ceramic blank temperature. It is enough to burn through the ceramic blank;
  • this embodiment adopts the horizontal rotary sintering technology of the cylindrical blank, that is, the ceramic membrane blank is sintered horizontally in the blast sintering furnace, and there is no rotation at 40°C, and the rotation speed is 2r at 40°C to 360°C /h, the speed is 3r/h during the cooling process;
  • a processing method for a ceramic modified PTFE film for a 5G high-frequency copper-clad laminate comprising the following steps:
  • Ceramic powder is subjected to high-temperature heat treatment, the particle diameter of described ceramic powder is D50 6um, heat treatment temperature is 600 °C, and heat treatment time is 24h;
  • the whole sintering process includes three stages of heating, heat preservation and cooling.
  • the heating stage and cooling stage need to be slow to ensure the uniformity of the ceramic blank temperature. It is enough to burn through the ceramic blank;
  • this embodiment adopts the horizontal rotary sintering technology of the cylindrical blank, that is, the ceramic membrane blank is sintered horizontally in the blast sintering furnace, and there is no rotation at 40°C, and the rotation speed is 3r at 40°C to 360°C /h, the speed is 4r/h during the cooling process;
  • all select micron order ceramic powder to prepare ceramic modified PTFE film (or ceramic filled PTFE film), preferred particle size 1um-6um ceramic powder, nanoscale ceramic powder same mass percentage ceramic powder volume-to-mass ratio can improve, not It is conducive to the dispersion of ceramic powder.
  • the addition of the same mass percentage of ceramic powder with a particle size higher than 6um cannot meet the required dielectric constant and dielectric loss. At the same time, the ceramic powder will fall off and form holes during film formation.
  • the heat treatment temperature used for high-temperature heat treatment of ceramic powder is 400°C-600°C, and the time is 24h-72h, to selectively remove surface coupling agents and other substances, retain some active groups, and avoid ceramic powder agglomeration and mixing process Not easy to disperse.
  • the high temperature dispersant is a titanate coupling agent.
  • the horizontal rotary sintering technology of the cylindrical blank is adopted.
  • the roller distance of the driving device for driving the blank to rotate is 400mm-700mm.
  • the blank does not rotate at 40°C, and the blank rotates at 1r/h at 40°C-360°C. ⁇ 3r/h, when cooling down, the blank rotation speed is 2r/h ⁇ 4r/h, to avoid residual stress in the XY direction of the copper clad laminate substrate film, and realize the preparation of ceramic modified PTFE films for high frequency copper clad laminates with a thickness of 0.015 ⁇ 10mm.
  • the polytetrafluoroethylene suspension resin preferably has a mass percentage of 65% to 95%
  • the ceramic powder preferably has a mass percentage of 4.5% to 30%
  • the high temperature dispersant preferably has a mass percentage of 0.5% to 5%.
  • the coefficient of thermal expansion can reach 15-30ppm/°C
  • the dielectric constant of single-layer and laminated films at 10GHz can be adjusted to 2.6-3.2
  • the loss factor is less than 0.0015.
  • the high heat treatment method of ceramic powder reduces the proportion of surface hydroxyl groups and improves the high High-frequency copper-clad laminates are resistant to CAF (conductive anode filament), and PCBs prepared using this ceramic-modified PTFE film meet the tracking resistance CTI>600V.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Materials Engineering (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Laminated Bodies (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)

Abstract

本发明公开了一种5G高频覆铜板用陶瓷改性PTFE薄膜的加工方法，包括：将陶瓷粉进行高温热处理；将上述处理后的陶瓷粉用筛网过筛，再将聚四氟乙烯悬浮树脂、陶瓷粉和高温分散剂进行混合；将上述混合后的混合料倒入模具中，压制成中空的圆柱形毛坯，圆柱形毛坯脱模后，得到陶瓷膜毛坯；将陶瓷膜毛坯放入鼓风烧结炉中进行烧结；将烧结好的陶瓷膜毛坯置于保温炉中保温，待陶瓷膜毛坯温度均匀后，从保温炉中取出陶瓷膜毛坯，在陶瓷膜毛坯的中心孔中顶入芯轴后，按照设定的薄膜厚度对陶瓷膜毛坯进行旋切，得到陶瓷改性PTFE薄膜。本发明可改善陶瓷粉分散的均匀性，成膜的膜厚均匀性、膜层均匀性好，可批量生产，加工难度小，实用性高。

Description

5G高频覆铜板用陶瓷改性PTFE薄膜的加工方法 技术领域
本发明属于高频及超高频无线通信技术领域，具体涉及一种5G高频覆铜板用陶瓷改性PTFE薄膜的加工方法，该陶瓷改性PTFE薄膜可作为高频覆铜板及多层高速覆铜板的基材使用。
背景技术
目前，陶瓷填充PTFE薄膜大多使用PTFE乳液，或分散PTFE树脂添加陶瓷粉，采用基础压延的方法制备陶瓷填充PTFE薄膜，由于加工难度大，所以对无机陶瓷进行表面改性，嫁接偶联剂，并在生产过程中添加其他助剂，且由于压辊精度、尺寸及乳液分散均匀性限制，使得基础PTFE乳液及分散PTFE树脂通常只能作为实验室研究使用，而且成膜的膜厚均匀性、膜层均匀性很难满足实际超过500mm宽幅的高频及超高频覆铜板用基材膜的使用，不能满足大批量生产的需要，因此实用性很低。
采用悬浮聚四氟乙烯制备陶瓷膜时,烧结时通常采用立式烧结方式，由于毛坯自重大，导致烧结后毛坯上下端尺寸差异过大(即出现大小头现象)，毛坯变形，导致车削薄膜时材料浪费较大，增加了成本。
发明内容
本发明所要解决的技术问题是针对上述现有技术的不足提供一种5G高频覆铜板用陶瓷改性PTFE薄膜的加工方法，本5G高频覆铜板用陶瓷改性PTFE薄膜的加工方法可改善陶瓷粉分散的均匀性，成膜的膜厚均匀性、膜层均匀性好，加工难度小，能满足大批量生产的需要，实用性高。
为实现上述技术目的，本发明采取的技术方案为：
一种5G高频覆铜板用陶瓷改性PTFE薄膜的加工方法，包括以下步骤：
(1)将陶瓷粉进行高温热处理；
(2)将上述处理后的陶瓷粉用筛网过筛，再将聚四氟乙烯悬浮树脂、陶瓷粉和高温分散剂进行混合；
(3)将上述混合后的混合料倒入模具中，压制成中空的圆柱形毛坯，圆柱形毛坯脱模后，得到陶瓷膜毛坯；
(4)将陶瓷膜毛坯放入鼓风烧结炉中进行烧结；
(5)将烧结好的陶瓷膜毛坯置于保温炉中保温，待陶瓷膜毛坯温度均匀后，从保温炉中 取出陶瓷膜毛坯，在陶瓷膜毛坯的中心孔中顶入芯轴后，按照设定的薄膜厚度对陶瓷膜毛坯进行旋切，得到陶瓷改性PTFE薄膜。
作为本发明进一步改进的技术方案，所述的步骤(1)具体为：
将陶瓷粉进行高温热处理，所述陶瓷粉的粒径为1um～6um，热处理温度为400℃～600℃，热处理时间为24h-72h。
作为本发明进一步改进的技术方案，所述的步骤(2)具体为：
将上述处理后的陶瓷粉用200目筛网过筛，再将聚四氟乙烯悬浮树脂、陶瓷粉和高温分散剂进行粗混，粗混后用混料机进行精混，其中混料机的筛网孔径为0.5mm～1.0mm，混料机的转速为1500r/min～3600r/min，混合次数为5遍～15遍。
作为本发明进一步改进的技术方案，所述步骤(2)中，所述聚四氟乙烯悬浮树脂的质量百分比为65％～95％，所述陶瓷粉的质量百分比为4.5％～30％，所述高温分散剂的质量百分比为0.5％～5％。
作为本发明进一步改进的技术方案，所述的步骤(3)具体为：
将上述精混后的混合料倒入模具中，压制成中空的圆柱形毛坯，压制压力为20MPa-30MPa，保压时间为1h-3h，30min后卸去压力，脱模，得到陶瓷膜毛坯，陶瓷膜毛坯的外径为560mm～580mm，轴向长度≥500mm。
作为本发明进一步改进的技术方案，所述的步骤(4)具体为：
所述陶瓷膜毛坯在烧结炉内卧式旋转烧结，40℃以下时，陶瓷膜毛坯无转动，40℃～360℃时，陶瓷膜毛坯的转速为1r/h～3r/h，降温过程中，陶瓷膜毛坯的转速为2r/h～4r/h。
作为本发明进一步改进的技术方案，所述的步骤(5)具体为：
将烧结好的陶瓷膜毛坯置于90-100℃的保温炉中保温，待陶瓷膜毛坯温度均匀后，从保温炉中取出陶瓷膜毛坯，在陶瓷膜毛坯的中心孔中顶入专用芯轴后，安装到旋切机上，按照设定的薄膜厚度对陶瓷膜毛坯进行旋切，得到陶瓷改性PTFE薄膜，其中陶瓷改性PTFE薄膜的厚度为0.1mm。
本发明的有益效果为：
1、本发明采用高热处理陶瓷粉方法选择性去除表面偶联剂等物质，保留部分活性基团，避免陶瓷粉结团混料过程中不好分散；降低表面羟基基团比例；提高了高频覆铜板抗CAF(导电性阳极丝)能力；使用本发明的陶瓷改性PTFE薄膜制备的PCB满足耐漏电痕性CTI>600V。
2、本发明在制备过程添加了高温分散剂，改善了陶瓷粉分散的均匀性，使用混料机将聚四氟乙烯悬浮树脂、陶瓷粉和高温分散剂共混，该混合方式均匀性好，可批量生产，加工难度小；本发明采用旋切成膜技术，可实现膜厚均匀，宽幅膜，实用性高；能满足实际超过500mm 宽幅的高频及超高频覆铜板用基材膜的使用。
3、本发明的陶瓷膜毛坯采用卧式旋转烧结技术，即圆柱形毛坯的轴线成水平状态，并以圆柱形毛坯的轴线为中心线在烧结炉内旋转烧结，避免了站立烧结容易出现大小头的弊端，烧结后毛坯外径上下大概相差5mm以内，车削薄膜时造成的材料损耗属于正常损耗。
具体实施方式
下面对本发明的具体实施方式做出进一步说明：
实施例1：
一种5G高频覆铜板用陶瓷改性PTFE薄膜的加工方法，包括以下步骤：
(1)将陶瓷粉进行高温热处理，所述陶瓷粉的粒径D50 1um，热处理温度为400℃，热处理时间为72h；
(2)将上述处理后的陶瓷粉用200目筛网过筛，再将聚四氟乙烯悬浮树脂、陶瓷粉和高温分散剂进行粗混，粗混后用立式锤磨混料机进行精混，其中立式锤磨混料机的筛网孔径为0.5mm，立式锤磨混料机的转速为1500r/min，混合次数为15遍；其中聚四氟乙烯悬浮树脂的质量百分比为95％，所述陶瓷粉的质量百分比为4.5％，所述高温分散剂的质量百分比为0.5％；
(3)将上述精混后的混合料倒入模具中，压制成中空的圆柱形毛坯，压制压力为20MPa，保压时间为1h，30min后卸去压力，脱模，得到陶瓷膜毛坯，陶瓷膜毛坯的外径为560mm，轴向长度≥500mm；
(4)将陶瓷膜毛坯放入鼓风烧结炉中进行烧结，整个烧结过程包括升温、保温、降温三个阶段，升温阶段、降温阶段均需缓慢，确保陶瓷毛坯温度的均匀性，保温时间要足够陶瓷毛坯烧透；本实施例采用筒状毛坯卧式旋转烧结技术，即陶瓷膜毛坯在鼓风烧结炉内卧式旋转烧结，40℃下无转动，40℃～360℃时，转速为1r/h，降温过程中转速为2r/h；
(5)将烧结好的陶瓷膜毛坯置于90℃的保温炉中保温，待陶瓷膜毛坯温度均匀后，从保温炉中取出陶瓷膜毛坯，在陶瓷膜毛坯的中心孔中顶入专用芯轴后，安装到旋切机上，按照设定的薄膜厚度和设置的车削速度对陶瓷膜毛坯进行旋切，得到陶瓷改性PTFE薄膜，其中陶瓷改性PTFE薄膜的厚度为0.1mm。
实施例2：
一种5G高频覆铜板用陶瓷改性PTFE薄膜的加工方法，包括以下步骤：
(1)将陶瓷粉进行高温热处理，所述陶瓷粉的粒径为D50 3um，热处理温度为500℃，热处理时间为48h；
(2)将上述处理后的陶瓷粉用200目筛网过筛，再将聚四氟乙烯悬浮树脂、陶瓷粉和高温分散剂进行粗混，粗混后用立式锤磨混料机进行精混，其中立式锤磨混料机的筛网孔径为0.8mm，立式锤磨混料机的转速为2000r/min，混合次数为10遍；所述聚四氟乙烯悬浮树脂的质量百分比为80％，所述陶瓷粉的质量百分比为17％，所述高温分散剂的质量百分比为3％；
(3)将上述精混后的混合料倒入模具中，压制成中空的圆柱形毛坯，压制压力为25MPa，保压时间为2h，30min后卸去压力，脱模，得到陶瓷膜毛坯，陶瓷膜毛坯的外径为570mm，轴向长度≥500mm；
(4)将陶瓷膜毛坯放入鼓风烧结炉中进行烧结，整个烧结过程包括升温、保温、降温三个阶段，升温阶段、降温阶段均需缓慢，确保陶瓷毛坯温度的均匀性，保温时间要足够陶瓷毛坯烧透；本实施例采用筒状毛坯卧式旋转烧结技术，即陶瓷膜毛坯在鼓风烧结炉内卧式旋转烧结，40℃下无转动，40℃～360℃时，转速为2r/h，降温过程中转速为3r/h；
(5)将烧结好的陶瓷膜毛坯置于90℃的保温炉中保温，待陶瓷膜毛坯温度均匀后，从保温炉中取出陶瓷膜毛坯，在陶瓷膜毛坯的中心孔中顶入专用芯轴后，安装到旋切机上，按照设定的薄膜厚度和设置的车削速度对陶瓷膜毛坯进行旋切，得到陶瓷改性PTFE薄膜，其中陶瓷改性PTFE薄膜的厚度为0.1mm。
实施例3：
一种5G高频覆铜板用陶瓷改性PTFE薄膜的加工方法，包括以下步骤：
(1)将陶瓷粉进行高温热处理，所述陶瓷粉的粒径为D50 6um，热处理温度为600℃，热处理时间为24h；
(2)将上述处理后的陶瓷粉用200目筛网过筛，再将聚四氟乙烯悬浮树脂、陶瓷粉和高温分散剂进行粗混，粗混后用立式锤磨混料机进行精混，其中立式锤磨混料机的筛网孔径为1.0mm，立式锤磨混料机的转速为3600r/min，混合次数为5遍；所述聚四氟乙烯悬浮树脂的质量百分比为65％，所述陶瓷粉的质量百分比为30％，所述高温分散剂的质量百分比为5％；
(3)将上述精混后的混合料倒入模具中，压制成中空的圆柱形毛坯，压制压力为30MPa，保压时间为3h，30min后卸去压力，脱模，得到陶瓷膜毛坯，陶瓷膜毛坯的外径为580mm，轴向长度≥500mm；
(4)将陶瓷膜毛坯放入鼓风烧结炉中进行烧结，整个烧结过程包括升温、保温、降温三个阶段，升温阶段、降温阶段均需缓慢，确保陶瓷毛坯温度的均匀性，保温时间要足够陶瓷毛坯烧透；本实施例采用筒状毛坯卧式旋转烧结技术，即陶瓷膜毛坯在鼓风烧结炉内卧式旋转烧结，40℃下无转动，40℃～360℃时，转速为3r/h，降温过程中转速为4r/h；
(5)将烧结好的陶瓷膜毛坯置于100℃的保温炉中保温，待陶瓷膜毛坯温度均匀后，从 保温炉中取出陶瓷膜毛坯，在陶瓷膜毛坯的中心孔中顶入专用芯轴后，安装到旋切机上，按照设定的薄膜厚度和设置的车削速度对陶瓷膜毛坯进行旋切，得到陶瓷改性PTFE薄膜，其中陶瓷改性PTFE薄膜的厚度为0.1mm。
上述实施例中，均选择微米级陶瓷粉制备陶瓷改性PTFE薄膜(或陶瓷填充PTFE薄膜)，优选粒径1um-6um陶瓷粉，纳米级陶瓷粉相同质量百分比陶瓷粉体积质量比会提高，不利于陶瓷粉分散，粒径高于6um陶瓷粉相同质量百分比添加达不到要求介电常数以及介质损耗，同时成膜时陶瓷粉会脱落形成孔洞。
上述实施例中，陶瓷粉进行高温热处理使用的热处理温度为400℃-600℃，时间24h-72h，选择性去除表面偶联剂等物质，保留部分活性基团，避免陶瓷粉结团混料过程中不好分散。
上述实施例中，高温分散剂为钛酸脂偶联剂。
上述实施例中，均采用筒状毛坯卧式旋转烧结技术，带动毛坯旋转的驱动装置的辊距为400mm～700mm，40℃下毛坯无转动，40℃～360℃时，毛坯转速为1r/h～3r/h，降温时，毛坯转速为2r/h～4r/h，避免覆铜板基材膜XY方向应力残余，实现厚度为0.015～10mm范围内高频覆铜板用陶瓷改性PTFE薄膜制备。
上述实施例中，聚四氟乙烯悬浮树脂优选质量百分比为65％～95％，陶瓷粉优选质量百分比为4.5％～30％，高温分散剂优选质量百分比为0.5％～5％。热膨胀系数可达到15-30ppm/℃，在10GHz单层及叠层膜的介电常数可调控为2.6～3.2，损耗因子小于0.0015，采用高热处理陶瓷粉方法降低表面羟基基团比例，提高了高频覆铜板抗CAF(导电性阳极丝)能力，使用该陶瓷改性PTFE薄膜制备的PCB满足耐漏电痕性CTI>600V。
本发明的保护范围包括但不限于以上实施方式，本发明的保护范围以权利要求书为准，任何对本技术做出的本领域的技术人员容易想到的替换、变形、改进均落入本发明的保护范围。

Claims (7)

  1. 一种5G高频覆铜板用陶瓷改性PTFE薄膜的加工方法，其特征在于：包括以下步骤：
    (1)将陶瓷粉进行高温热处理；
    (2)将上述处理后的陶瓷粉用筛网过筛，再将聚四氟乙烯悬浮树脂、陶瓷粉和高温分散剂进行混合；
    (3)将上述混合后的混合料倒入模具中，压制成中空的圆柱形毛坯，圆柱形毛坯脱模后，得到陶瓷膜毛坯；
    (4)将陶瓷膜毛坯放入鼓风烧结炉中进行烧结；
    (5)将烧结好的陶瓷膜毛坯置于保温炉中保温，待陶瓷膜毛坯温度均匀后，从保温炉中取出陶瓷膜毛坯，在陶瓷膜毛坯的中心孔中顶入芯轴后，按照设定的薄膜厚度对陶瓷膜毛坯进行旋切，得到陶瓷改性PTFE薄膜。
  2. 根据权利要求1所述的5G高频覆铜板用陶瓷改性PTFE薄膜的加工方法，其特征在于：所述的步骤(1)具体为：
    将陶瓷粉进行高温热处理，所述陶瓷粉的粒径为1um～6um，热处理温度为400℃～600℃，热处理时间为24h-72h。
  3. 根据权利要求2所述的5G高频覆铜板用陶瓷改性PTFE薄膜的加工方法，其特征在于：所述的步骤(2)具体为：
    将上述处理后的陶瓷粉用200目筛网过筛，再将聚四氟乙烯悬浮树脂、陶瓷粉和高温分散剂进行粗混，粗混后用混料机进行精混，其中混料机的筛网孔径为0.5mm～1.0mm，混料机的转速为1500r/min～3600r/min，混合次数为5～15遍。
  4. 根据权利要求3所述的5G高频覆铜板用陶瓷改性PTFE薄膜的加工方法，其特征在于：所述步骤(2)中，所述聚四氟乙烯悬浮树脂的质量百分比为65％～95％，所述陶瓷粉的质量百分比为4.5％～30％，所述高温分散剂的质量百分比为0.5％～5％。
  5. 根据权利要求3所述的5G高频覆铜板用陶瓷改性PTFE薄膜的加工方法，其特征在于：所述的步骤(3)具体为：
    将上述精混后的混合料倒入模具中，压制成中空的圆柱形毛坯，压制压力为20MPa-30MPa，保压时间为1h-3h，30min后卸去压力，脱模，得到陶瓷膜毛坯，陶瓷膜毛坯的外径为560mm～580mm，轴向长度≥500mm。
  6. 根据权利要求5所述的5G高频覆铜板用陶瓷改性PTFE薄膜的加工方法，其特征在于：所述的步骤(4)具体为：
    所述陶瓷膜毛坯在烧结炉内卧式旋转烧结，40℃以下时，陶瓷膜毛坯无转动，40℃～360℃时，陶瓷膜毛坯的转速为1r/h～3r/h，降温过程中，陶瓷膜毛坯的转速为2r/h～4r/h。
  7. 根据权利要求6所述的5G高频覆铜板用陶瓷改性PTFE薄膜的加工方法，其特征在于：所述的步骤(5)具体为：
    将烧结好的陶瓷膜毛坯置于90-100℃的保温炉中保温，待陶瓷膜毛坯温度均匀后，从保温炉中取出陶瓷膜毛坯，在陶瓷膜毛坯的中心孔中顶入专用芯轴后，安装到旋切机上，按照设定的薄膜厚度对陶瓷膜毛坯进行旋切，得到陶瓷改性PTFE薄膜，其中陶瓷改性PTFE薄膜的厚度为0.1mm。
PCT/CN2022/086689 2021-05-22 2022-04-13 5g高频覆铜板用陶瓷改性ptfe薄膜的加工方法 WO2022247508A1 (zh)

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CN117565438A (zh) * 2024-01-16 2024-02-20 山东东岳高分子材料有限公司 一种磨砂表面的聚四氟乙烯薄膜的制备方法和应用
CN117565438B (zh) * 2024-01-16 2024-04-16 山东东岳高分子材料有限公司 一种磨砂表面的聚四氟乙烯薄膜的制备方法和应用

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