CN110372980A - A kind of low water absorption, high copper foil adhesive force PTFE ceramic composite substrate production method - Google Patents
A kind of low water absorption, high copper foil adhesive force PTFE ceramic composite substrate production method Download PDFInfo
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- CN110372980A CN110372980A CN201910635596.5A CN201910635596A CN110372980A CN 110372980 A CN110372980 A CN 110372980A CN 201910635596 A CN201910635596 A CN 201910635596A CN 110372980 A CN110372980 A CN 110372980A
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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
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- C—CHEMISTRY; METALLURGY
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- C08K7/00—Use of ingredients characterised by shape
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- 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
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The present invention relates to the production methods of a kind of low water absorption, the PTFE ceramic composite substrate of high copper foil adhesive force, include the following steps: that ceramic packing, coupling agent, water, dispersing agent are added in the high-speed mixer equipped with zirconia ball by a. according to a certain ratio, high-speed stirred 30 ~ 120 minutes, ceramic slurry is made;B. the ceramic packing that surface has been modified is made in ceramic slurry；C. first PTFE emulsion, dispersing agent, defoaming agent are stirred at low speed 3 ~ 15 minutes according to a certain ratio, then ceramic packing obtained in above-mentioned steps b is added in slurry according to a certain ratio, then high-speed stirred 30 ~ 60 minutes, return again to progress deaeration processing in low-speed mixer；D. the slurry of above-mentioned steps c is transported in the steeping vat of gluing machine with diaphragm pump；E. PP piece is made in glass fabric；F. pp piece makes PTFE ceramic composite substrate in step e.The invention enables the better performances of PTFE ceramic composite substrate.
Description
Technical field
The present invention relates to the production methods of a kind of low water absorption, the PTFE ceramic composite substrate of high copper foil adhesive force, belong to
High-frequency copper-clad plate field used in microwave circuit.
Background technique
In recent years, the fast development of the communication technology, especially the 5G communication technology initially enter the commercialization stage, high frequency,
The increasingly huge increasing of the demand of high speed copper-clad plate brings very big impact, the pcb board of traditional FR-4 to traditional PCB copper-clad plate
It will be unable to meet the requirement of 5G communication, the exploitation of high frequency composite substrate of a kind of low cost, high-performance, high stable seems especially heavy
It wants.In recent years, scientific worker is to influence of the materials such as resin, filler, coupling agent of high frequency, high speed baseplate material to substrate
It is extensively and profoundly studied, and proposes a variety of high performance high frequency composite substrate production methods to meet communication technology reality
The requirement used.But practical application is few at home, and the field is mainly dominated by the U.S. in the world, and wherein Rogers is occupied
60% or more the market share is sought entirely.
The design feature of PTFE has high stability and outstanding microwave electric property: low-k, low dielectric loss,
And dielectric constant and dielectric loss are unobvious with the raising variation of frequency.Therefore PTFE is highly suitable for as high speed, height
The matrix resin of the baseplate material of frequency.PTFE non-stick and Z-direction thermal expansion coefficient it is big, the thermal expansion system with copper
Number difference is larger, easily causes in thermal histories bad with copper foil engaging force, causes copper foil adhesive force low, national military standard high-frequency copper-clad plate
Copper foil peeling force Yao Qiu≤1.5N/mm.At present be generally used inorganic filler (SiO2, TiO2, Al2O3, MgTiO3,
BaTiO3 etc.) addition improve the thermal expansion coefficient of PTFE.
The structure feature of the high stability of PTFE causes PTFE to have inertia, is not easy in conjunction with other objects.Therefore it easily causes
Ceramic packing and PTFE binding force are small, and intermiscibility is poor, cause the water absorption rate index of PTFE ceramic composite substrate poor, easily moist,
The stabilization of substrate is influenced, and is remarkably decreased the microwave property of substrate, especially dielectric loss.Generally using coupling agent to filler
Surface is modified, to improve filler and the interface intermiscibility of PTFE.Stuffing surface modification mainly have surface chemistry coating modification method,
The modified method of precipitation reaction method, mechanical-chemical modification method, chemical graft, composite modified method etc..In high frequency composite substrate field one
As using surface chemistry coating modification method is changed, this method mainly has two techniques: dry process and wet processing.
Inorganic filler is added in PTFE, and scientific worker does many research.Wherein patent ZL20140376656.3 is public
It has opened by the way that low speed ball milling, heat zone are suppressed again after being mixed and dried fluororesin powder, inorganic filler, water and zirconium oxide bead
The water absorption rate of PTFE copper-clad plate, PTFE copper-clad plate made from the method is larger (0.15%).Patent CN201410376691.5 is disclosed
Fluororesin cream, inorganic filler and thickener are mixed, are coated on the substrate that can be release, baking, heat zone are passed through
The compound Jie's substrate of PTFE is suppressed to obtain, the water absorption rate of this substrate is larger (0.15%), and peel strength of copper foil is smaller (1.53N/mm).Specially
Sharp ZL201610545312.X is disclosed to be mixed by PTFE resin, silica, high dielectric constant filler, fire retardant, water etc.
PTFE medium substrate is made, peel strength of copper foil is smaller (1.31N/mm).The filler that its main cause is added does not carry out table
Face is modified, i.e., filler surface is hydrophily, and the surface PTFE is hydrophobicity, and two all joint interfaces deposit immiscible property, therefore easily make
At there is two socket part position to generate stomata, especially substrate surface stomata, the water absorption rate of substrate and the adhesive force of copper foil can be seriously affected.
And to improve the surface pores of substrate, it first has to solve the problems, such as mixing for filler and the interface PTFE, generally uses surface chemistry packet
Cover modification, i.e., powder be modified using coupling agent, make coupling agent hydrophilic radical with filler surface in conjunction with, hydrophobic grouping and
The surface PTFE combines, from the intermiscibility for then reaching the two interface.So the cladding integrality and idol of coupling agent and filler surface
The intensity of connection agent and filler engaging force is to influence two key factors of substrate water absorption rate.
Summary of the invention
The shortcomings that the purpose of the present invention is overcoming the prior art and deficiency, provide a kind of low water absorption, high copper foil adhesive force,
Meet the production method of the PTFE ceramic composite substrate of environmental requirement.
In order to achieve the above-mentioned object of the invention, present invention employs technical solutions below:
A kind of low water absorption, high copper foil adhesive force PTFE ceramic composite substrate production method, the production technology include with
Under several steps:
A. ceramic packing, coupling agent, water, dispersing agent are added to according to a certain ratio in the high-speed mixer equipped with zirconia ball,
High-speed stirred 30 ~ 120 minutes, ceramic slurry is made;
B. ceramic slurry is added to pelletizer by diaphragm pump and carries out mist projection granulating, the ceramic packing that surface has been modified is made；
C. first PTFE emulsion, dispersing agent, defoaming agent are added to according to a certain ratio in high-speed mixer and are stirred at low speed 3 ~ 15 minutes,
Ceramic packing obtained in above-mentioned steps b is added in slurry again, then high-speed stirred 30 ~ 60 minutes according to a certain ratio, then turned
Deaeration processing is carried out into low-speed mixer；
D. the slurry of above-mentioned steps c is transported in the steeping vat of gluing machine with diaphragm pump；
E. PP piece is made by vertical gluing machine dipping, drying, winding in glass fabric；
F. in step e pp piece it is cut, with piece, lamination, weighing, after lamination, in the vacuum press through vacuum, high pressure, high temperature item
Part auto-stitching makes PTFE ceramic composite substrate.
Preferably, the weight percent composition of the ceramic slurry: 50% ~ 80% ceramic packing, 20% ~ 50%
Water, 0.5 ~ 5% coupling agent, 0.3 ~ 1% dispersing agent, the sum total of each component are 100%；The weight percent of the slurry forms:
20% ~ 50% ceramic packing；50% ~ 80% PTFE emulsion；0 ~ 1% dispersing agent, the sum total of each component are 100%.
Preferably, the inlet temperature of the ceramic slurry mist projection granulating is 200 DEG C ~ 250 DEG C, and outlet temperature is
100 DEG C ~ 130 DEG C, 8000 turns of atomizer rotating speed ~ 15000 turns/min.
Preferably, the oven temperature of the gluing machine is 250 DEG C ~ 420 DEG C, speed: 1.5 ~ 6m/min；It is described true
The pressure of air compressor machine is 3 ~ 9MPa, and temperature is 350 ~ 400 DEG C, and vacuum degree is 60 ~ 180 points of high-temperature holding time less than -0.1MPa
Clock starts to add half pressure when temperature is raised to 310 DEG C ~ 325 DEG C, and total pressure is added when temperature, which reaches a high temperature, to be kept the temperature, and temperature-fall period is protected
Hold half pressure.
Present invention employs ceramic packings first with coupling agent wet-mixing at slurry, this step preferably resolves coupling agent
With the surface coated integrality of filler；The ceramic packing that surface has been modified is made by making material mode by spraying in slurry again, this
Mainly there are three purposes for step: first has been drying functions；Second is chemically reacted for coupling agent and ceramic packing surface
Energy is provided, to solve the problems, such as ceramic packing and coupling agent bond strength；Third is the high speed rotation of logical pelletizer atomizing disk
Turn the problems such as can reach granular size (uniform), grain shape (ball-type) and distribution of particles (concentration) that control money filler is reunited,
Make ceramic packing that there is preferable mobility；Again be uniformly mixed ceramic packing, PTFE emulsion, dispersing agent, defoaming agent and water etc.,
Dipping, gluing, high-temperature vacuum, which are laminated, is made PTFE ceramic composite substrate.The production method can realize that PTFE ceramic composite substrate has
Some dielectric constant seriations (2.6 ~ 10.2), low-dielectric loss, low water absorption, low thermal coefficient of expansion, high copper foil adhesive force etc.
Function.
Detailed description of the invention
Fig. 1 is the filler production technological process of PTFE ceramic composite substrate of the invention；
Fig. 2 is the production technological process of PTFE ceramic composite substrate of the invention.
Specific embodiment
The embodiment of the present invention is described below in detail, examples of the embodiments are shown in the accompanying drawings, wherein from beginning to end
Same or similar label indicates same or similar element or element with the same or similar functions.Below with reference to attached
The embodiment of figure description is exemplary, it is intended to is used to explain the present invention, and is not considered as limiting the invention.
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that described herein, specific examples are only used to explain the present invention, not
To limit the present invention.
As depicted in figs. 1 and 2, the PTFE Ceramic Composite base of a kind of low water absorption proposed by the present invention, high copper foil adhesive force
Plate can be achieved as follows:
As depicted in figs. 1 and 2, the first step, ceramic packing, coupling agent, water, dispersing agent by weight (50 ~ 80% ceramic packing,
20 ~ 50% water, 0 ~ 5% coupling agent, 0 ~ 1% dispersing agent, comprehensive each component is 100%) to weigh up；By ceramic packing: zirconium oxide
Ball weight ratio are as follows: 1:1.5 ~ 3 weigh up zirconia ball.
It is mixed 1 ~ 3 hour in vertical mixer, uniformly mixed slurry crosses 120 mesh ~ 240 mesh sieve, and with conveying
It is stand-by that the modified powder in ceramic packing surface is made after drying into mist projection granulating.Its atomizing granulating technology parameter are as follows: inlet temperature
It is 200 DEG C ~ 250 DEG C, outlet temperature is 100 DEG C ~ 130 DEG C, 8000 turns of atomizer rotating speed ~ 15000 turns/min.
Second step, by weight by ceramic packing obtained above, PTFE emulsion, dispersing agent etc. are as follows: 20% ~ 50% ceramics
Filler；50% ~ 80% PTFE emulsion；0 ~ 1% dispersing agent equal proportion weighs, first by the PTFE emulsion prepared, additive, idol
Connection agent, which is added in high-speed mixer, to be stirred at low speed 3 ~ 15 minutes, then high-speed stirred 30 ~ 60 minutes, is returned again in low-speed mixer
Deaeration processing is carried out, is made etc. and to use slurry.(high-speed mixer stirs at low speed speed: 800 ~ 1000N/min；High-speed mixer is high
Fast mixing speed: 1000 ~ 2500N/min;50 ~ 800N/min of low-speed mixer speed) stand-by slurry is made.
The above-mentioned slurry that makes is injected in the steeping vat of gluing machine, then glass fabric is passed through vertical gluing by third step
Impregnation is carried out in the steeping vat of machine, then by frictioning metering roll control gluing thickness, is entered back into the baking oven of vertical gluing machine
Dried (oven temperature: 250 DEG C ~ 420 DEG C, speed: 1.5 ~ 6m/min), obtain PP piece.
4th step, above-mentioned pp piece is cut, with piece, lamination, after weighing with steel plate after copper foil, aluminium foil, pressure, buffer board,
Carrier combination, by vacuum press, in vacuum, high pressure, hot conditions auto-stitching, (pressure is 3 ~ 9MPa;Temperature be 350 ~
400℃;Vacuum degree is less than -0.1MPa;High-temperature holding time 60 ~ 180 minutes;Start when temperature is raised to 310 DEG C ~ 325 DEG C
Add half pressure;Add total pressure when temperature, which reaches a high temperature, to be kept the temperature;Temperature-fall period keeps half to press), then cooling tears plate open and obtains copper-clad plate,
Copper-clad plate obtains PTFE ceramic composite substrate of the invention after cutting according to required load.
The present invention that the present invention is formed using above-mentioned formula and technique, can be obtained the dielectric constant of PTFE ceramic composite substrate
2.65 ~ 10.2 series, low dielectric loss (≤0.002), low water absorption (≤0.03%), high copper foil adhesive force (≤2.5N/mm) property
Energy index fully meets the requirement for meeting communication technology actual use.And the present invention also has the following characteristics that
1. ceramic packing, coupling agent, water, dispersing agent etc. mix, can real coupling agent and ceramic packing surface uniform cladding.Lead to again
The combination of functional group of ceramic packing and coupling agent can be realized by crossing mist projection granulating mode, while be can also be achieved pottery money filler and being atomized
In the case of by surface tension of liquid presence, be in spherical, the dry glomeration in the case where being granulated hot wind using droplet, make to be modified
Ceramic packing has good mobility.This mode can realize that two kinds of coupling agent wet process, dry method technological advantages combine.To reduce
The water absorption rate of ceramic packing itself.
2. the energy Quick uniform dispersion in PTFE emulsion of the modified ceramic filler as made from being granulated, is mainly filled out by ceramics
The ball-type reason of material causes to flow, filler particles distribution is concentrated, be between ceramic filler particles it is soft-agglomerated, coupling agent it is hydrophilic
Functional group is dredged in functional group's draining and there is row and tear open in conjunction with ceramic packing surface, so that ceramic packing be caused to be easier to disperse
Uniformly.Make PTFE by coupling agent bridge joint can preferable coating ceramic filler, to reduce the water absorption rate of PTFE composite substrate.
3. formula of size system of the present invention has, stabilization, viscosity is adjustable controllably, is uniformly dispersed and using water as primary solvent
Meet environmental requirement.
4. the present invention proposes that high-temperature vacuum processes parameter is the analysis of DSC, TGA in conjunction with PP piece as a result, starting in PTFE
By pressurization when there is softening point, PTFE is improved with ceramic packing, glass-fiber-fabric three and combines degree, to improve PTFE
The copper foil adhesive force of composite substrate.
5. material technology of the present invention is simple, stablizes, favorable reproducibility.
6. material of the present invention has been applied to produce, can be prepared in wireless telecommunications with the PTFE Ceramic Composite high-frequency copper-clad plate
The devices such as high-precision antenna, LNB wiring board, phase shifter, power splitter, wearable antenna, radar, car antenna.
It should be pointed out that above embodiments are only representative examples of the invention.The present invention can also there are many deformations.It is all
Any simple modification, equivalent change and modification to the above embodiments of essence according to the present invention are considered as belonging to this
The protection scope of invention.
Claims (4)
1. the production method of the PTFE ceramic composite substrate of a kind of low water absorption, high copper foil adhesive force, it is characterized in that: the production
Technique includes following steps:
A. ceramic packing, coupling agent, water, dispersing agent are added to according to a certain ratio in the high-speed mixer equipped with zirconia ball,
High-speed stirred 30 ~ 120 minutes, ceramic slurry is made;
B. ceramic slurry is added to pelletizer by diaphragm pump and carries out mist projection granulating, the ceramic packing that surface has been modified is made；
C. first PTFE emulsion, dispersing agent, defoaming agent are added to according to a certain ratio in high-speed mixer and are stirred at low speed 3 ~ 15 minutes,
Ceramic packing obtained in above-mentioned steps b is added in slurry again, then high-speed stirred 30 ~ 60 minutes according to a certain ratio, then turned
Deaeration processing is carried out into low-speed mixer；
D. the slurry of above-mentioned steps c is transported in the steeping vat of gluing machine with diaphragm pump；
E. PP piece is made by vertical gluing machine dipping, drying, winding in glass fabric；
F. in step e pp piece it is cut, with piece, lamination, weighing, after lamination, in the vacuum press through vacuum, high pressure, high temperature item
Part auto-stitching makes PTFE ceramic composite substrate.
2. the production method of the PTFE ceramic composite substrate of low water absorption according to claim 1, high copper foil adhesive force,
It is characterized in that: the weight percent composition of the ceramic slurry: 50% ~ 80% ceramic packing, 20% ~ 50% water, 0.5 ~ 5%
Coupling agent, 0.3 ~ 1% dispersing agent, the sum total of each component are 100%；The weight percent of the slurry forms: 20% ~ 50% pottery
Porcelain filling；50% ~ 80% PTFE emulsion；0 ~ 1% dispersing agent, the sum total of each component are 100%.
3. the production method of the PTFE ceramic composite substrate of low water absorption according to claim 1, high copper foil adhesive force,
Be characterized in that: the inlet temperature of the ceramic slurry mist projection granulating is 200 DEG C ~ 250 DEG C, and outlet temperature is 100 DEG C ~ 130 DEG C, mist
Change 8000 turns of device revolving speed ~ 15000 turns/min.
4. the production method of the PTFE ceramic composite substrate of low water absorption according to claim 1, high copper foil adhesive force,
Be characterized in that: the oven temperature of the gluing machine is 250 DEG C ~ 420 DEG C, speed: 1.5 ~ 6m/min；The pressure of the vacuum press
For 3 ~ 9MPa, temperature is 350 ~ 400 DEG C, and vacuum degree is high-temperature holding time 60 ~ 180 minutes less than -0.1MPa, when temperature liter
Start when to 310 DEG C ~ 325 DEG C plus half pressure, total pressure is added when temperature, which reaches a high temperature, to be kept the temperature, temperature-fall period keeps half to press.
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Cited By (2)
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| CN111216427A (en) * | 2019-12-02 | 2020-06-02 | 珠海国能新材料股份有限公司 | Preparation method of ceramic-filled PTFE (polytetrafluoroethylene) copper-clad plate |
| CN113365429A (en) * | 2020-04-21 | 2021-09-07 | 广州市东泓氟塑料股份有限公司 | High-frequency high-speed copper-clad plate with good dielectric constant consistency and preparation and application thereof |
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