CN109910400A - The curtain coating preparation method of microwave complex media plate and microwave complex media plate obtained - Google Patents
The curtain coating preparation method of microwave complex media plate and microwave complex media plate obtained Download PDFInfo
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Abstract
The present invention discloses a kind of curtain coating preparation method of microwave complex media plate, it is related to microwave complex media plate technique field, there is the problem of high cost, high pollution based on existing microwave complex media plate impregnation technology and propose, the present invention is the following steps are included: (1) prepares casting films glue；(2) it is cast；(3) transmission drying；(4) it demoulds；(5) it post-processes；(6) lamination matches；The present invention also provides one kind microwave complex media plate as made from above-mentioned preparation method；The beneficial effects of the present invention are: the microwave complex media plate core plate being prepared is uniform system, and ceramic powder is evenly distributed among PTFE matrix, and dielectric properties isotropism is good, copper foil adhesive force is high；Preparation method is simple, avoids the sewage collecting of impregnation technology and handles and discharge, green energy conservation meets environmental requirement.
Description
Technical field
The present invention relates to microwave complex media plate technique fields, and in particular to a kind of curtain coating preparation of microwave complex media plate
Method and microwave complex media plate obtained.
Background technique
As electronics and IT products develop to high speed, multi-functional, large capacity and portable low consumption direction, traditional FR4 (ring
Oxygen resin) substrate is unable to satisfy its requirement, gradually substituted by the microwave composite medium substrate of high speed, high reliability.It is poly-
Tetrafluoroethene (PTFE) material, which has, is lost that low, dielectric constant is stable, chemical stability is high, water absorption rate is low and good weatherability etc. is all
More advantages, using its as the microwave complex media plate of basis material be widely used in 300MHz~40GHz wave band it is airborne, spaceborne,
The high bands such as missile-borne, carrier-borne and condition of badly installing.
Although PTFE has excellent electric property, since its glass transition temperature (Tg) is very low, rigidity is very poor, mechanical
Intensity is inadequate, this just determines that its processing conditions is very harsh, seriously affects the use reliability of microwave complex media.Therefore,
It is one of the scheme for solving problem above that glass fiber reinforced materials are added in PTFE substrate.Current PTFE base microwave both at home and abroad is compound
Dielectric-slab commodity mainly have micro- glass and a glass-fiber-fabric and ceramic powder two major classes type, fiberglass reinforced microwave complex media plate it is main
Preparation method is wet impregnation technique, i.e., PTFE emulsion dipping glass-fiber-fabric manufactures the method that glass varnished cloth is then superimposed hot pressing.Leaching
Stain method mainly uses vertical glue dipping machine.Vertical glue dipping machine height is 10m or more, considers that heat dissipation and heat transfer, usual workshop setting are high
Degree is 20m or so, very high to workshop setting requirements.The impregnation process of vertical glue dipping machine is also related to the transmission of multistep roller and thickness measure
Function, the device is complicated, investment is larger.In addition, to the pretreatment of raw material, the mixed configuration of glue, discharge of discarded glue etc.
Process generates a large amount of waste water, needs to carry out ability normal discharge after secondary treatment.It, should with the raising to environmental protection degree
Kind technique, which will meet urban environmental protection requirement, must be provided with complicated process, and manufacturing cost is high.
Therefore, a kind of simple process, at low cost, clean and environmental protection are found, while it is multiple to have excellent performance stable PTFE base microwave
Closing dielectric-slab preparation method is current urgent problem to be solved.
Summary of the invention
The technical issues of solution of the invention, is that existing microwave complex media plate impregnation technology has high cost, high dirty
The problem of dye.
The present invention adopts the following technical solutions solves above-mentioned technical problem:
The present invention provides a kind of curtain coating preparation method of microwave complex media plate, comprising the following steps:
(1) casting films glue is prepared；
(2) it is cast: the casting films glue prepared in step (1) is placed in casting machine, obtain casting films；
(3) transmission drying: casting films obtained in step (2) are dried by drying oven；
(4) it demoulds: after casting films obtained in step (3) are cooled to room temperature, obtaining microwave composite dielectric film；
(5) it post-processes: the microwave composite dielectric film obtained in step (4) is subjected to plasma activation processing；
(6) lamination matches: using treated in step (5) microwave composite dielectric film as basic unit, with fluorine resin film
Overlapping matching, is overlapped, places metal foil respectively in superimposed top layer and bottom, and vacuum pressure is carried out in high temperature laminating machine
It closes, obtains microwave complex media plate.
Preferably, the casting films glue is made of the raw material of following weight fraction: 100 parts of PTFE emulsion solid content, fluorine
1~10 part of modifier, 100~400 parts of micro-ceramic powder, 0.1~4 part of surface modifier, hydrolysising solvent 0.08~5
Part, 0.5~15 part of auxiliary agent, 50~100 parts of solvent.
Preferably, the casting films glue the preparation method comprises the following steps:
(a) pretreatment of raw material: coupling agent is pre-processed by hydrolysising solvent and is hydrolyzed, and after ceramic powder is added, is placed in ball mill；
(b) wet-mixing: material, solvent, auxiliary agent, PTFE emulsion, the fluororesin modified dose of addition height in ball mill are cut
It cuts in stirred tank, is stirred under the conditions of 60-80 DEG C.
Preferably, the edge of a knife of casting machine is heated to 30-70 DEG C, the casting films glue prepared in step (1) is transferred to
Storage tank is heated to 30-70 DEG C by the storage tank of casting machine.
Preferably, the temperature of the drying oven is 130~170 DEG C, and drying time is 0.5~3h.
Preferably, before microwave composite dielectric film carries out plasma activation processing, microwave composite dielectric film is cut into
The thin slice of 1.1m × 1.3m.
Preferably, the condition of the plasma activation processing is N2: H2=0.4~0.8, flow be 800mL/min~
1200mL/min, power are 1600W~2200W, handle 35min~70min.
Preferably, the metal foil by one of copper, brass, aluminium, nickel or a variety of is made.
Preferably, the fluorine resin film is one of polytetrafluoroethylene (PTFE), perfluoroalkoxy resin, perfluoroethylene-propylene
Or a variety of compoundings.
Preferably, the fluorine resin film with a thickness of 0.0013mm~0.02mm.
Preferably, the condition of vacuum pressing-combining is carried out in high temperature laminating machine are as follows: 350~390 DEG C, 25~100Kg/cm2Under
2~10h of hot pressing.
Preferably, the hydrolysising solvent is one of water, methylene chloride, ethyl alcohol, acetone, propylene glycol monomethyl ether, dimethylbenzene
Or a variety of compoundings.
Preferably, the surface modifier is silane coupling agent, and the silane coupling agent is Z-6030, Z-6020, Z-
6040, one of Z-6124, Z-6011, Z-6076, Z-6032 or a variety of compoundings.
Preferably, the grain diameter of the micro-ceramic powder is 0.1~30 μm.
Preferably, the micro-ceramic powder is SiO2、TiO2、Al2O3、CaTiO3、SrTiO3、BaTiO3、AlN、BN、
One of SiC or a variety of compoundings.
Preferably, the partial size of particle is 0.1~1 μm in the PTFE emulsion.
Preferably, described fluororesin modified dose be perfluoroethylene-propylene, perfluoroalkoxy resin, ethylene-tetrafluoroethylene it is total
One or more of polymers, ethylene-chlorotrifluoro-ethylene copolymer compounding.
Preferably, the solvent is that one or more of water, 1,2-PD, methylene chloride, ethyl alcohol, acetone etc. are multiple
Match.
Preferably, the auxiliary agent is one or more of formic acid, polyetherimide, polyacrylamide compounding.
Preferably, the Ball-milling Time in the step (a) is 1~2h.
Preferably, the mixing time of high shear stirred tank is 30~120min, stirring rate 300 in the step (b)
~500r/min.
The present invention also provides one kind microwave complex media plate as made from above-mentioned preparation method.
The beneficial effects of the present invention are:
(1) the microwave complex media copper-clad plate core plate being prepared in the present invention is uniform system, and ceramic powder is uniformly distributed
Among PTFE matrix, dielectric properties isotropism is good, copper foil adhesive force is high；
(2) it is formulated in the preparation process of microwave complex media plate of the present invention simply, almost without waste water is generated, avoids impregnating
The sewage collecting of technique and processing and discharge, only generate a small amount of gas in sintering and hot pressing in the process, are not required to substantially
Gas sampling and processing are wanted, green energy conservation meets environmental requirement；
(3) the preparation process occupation area of equipment of microwave complex media plate is small in the present invention, and device fabrication is mature, technique road
Line is simple and fast, and condition is easily-controllable；Preparation cost is low, saves manpower financial capacity, stable product quality.
Detailed description of the invention
Fig. 1 is preparation technology flow chart of the invention；
Specific embodiment
The present invention is described in further details below with reference to Figure of description and embodiment.
Test material as used in the following examples, reagent, instrument and equipment etc. unless otherwise specified can be from business ways
Diameter obtains.
Embodiment 1
Table 1 is each component content in embodiment 2- embodiment 4:
Embodiment 2
According to each component content in 1 table of embodiment, microwave complex media plate is prepared, comprising the following steps:
(1) hydrolysising solvent is added in coupling agent Z-6040, stirs evenly, with melt of si O2Ball mill is added together,
1h is stirred in 60 DEG C of ball mill；
(2) after being cooled to room temperature, by whole materials, water, auxiliary agent, polytetrafluoroethylene (PTFE) (PTFE) lotion, poly- in ball mill
Perfluoroethylene-propylene (copolymer) (FEP) is added in high shear agitation kettle, stirs 30min in 60 DEG C of speed with 300r/min, setting is true
Empty deaeration mode obtains casting films glue；Wherein bonding force can be improved for fluororesin modified dose, micro-ceramic powder is filled out for enhancing
Material, water lytic agent is for cooperating coupling reaction, and auxiliary agent is used for gelatin viscosity stability, and solvent is adjusted for gelatin viscosity；
(3) edge of a knife of casting machine is heated to 40 DEG C, casting films glue is transferred to the storage tank of casting machine, by storage tank
It is heated to 40 DEG C, control edge of a knife slit width is 0.3mm, knife-band gap is 0.3mm, speed of service 2.5m/min, allows mixed solution
The curtain coating edge of a knife is flowed into start casting machine after full of the edge of a knife, smooth film is scraped on stainless steel band；
(4) by casting films obtained in step (3) under the transmission of stainless steel band, pass through drying oven, baking oven air blower
It opens, temperature setting is 130 DEG C, time 0.5h；
(5) it by the cooling 10min of casting films obtained in step (4), obtains with a thickness of 0.025mm, uniform, surface is smooth
Casting films, casting films are taken off from stainless steel band, produce continuous film with automatic coiling machine；
(6) microwave continuous composite dielectric film obtained in step (5) is cut into the thin slice of 1.1m × 1.3m；
(7) thin slice tow sides obtained in step (6) are subjected to plasma activation processing (state China GH-PM14), processing
Condition is gas ratio (N2: H2)=0.4, flow 800mL/min, power 1600W, time 35min；
(8) by treated in step (7) thin slice, the PTFE film of a 0.013mm is respectively placed in two sides up and down, as
Basic unit overlap 5, place electrolytic copper foil respectively in superimposed top layer and bottom, in high temperature laminating machine (Burkle) into
Row vacuum pressing-combining, pressing condition are 380 DEG C and 50Kg/cm2Lower hot pressing 5h obtains microwave complex media plate.
Embodiment 3
According to each component content in 1 table of embodiment, microwave complex media plate is prepared, comprising the following steps:
(1) hydrolysising solvent is added in coupling agent Z-6040, Z-6124, stirs evenly, with melt of si O2、TiO2Together plus
Enter ball mill, stirs 1.5h in 70 DEG C of ball mill；
(2) after being cooled to room temperature, by whole materials, water, auxiliary agent, polytetrafluoroethylene (PTFE) (PTFE) lotion, complete in ball mill
Fluoroalkyloxy resin (PFA) is added in high shear agitation kettle, stirs 60min, setting in 70 DEG C of speed with 400r/min
Vacuum defoamation mode obtains casting films glue；Wherein bonding force can be improved for fluororesin modified dose, micro-ceramic powder is for enhancing
Filler, water lytic agent is for cooperating coupling reaction, and auxiliary agent is used for gelatin viscosity stability, and solvent is adjusted for gelatin viscosity；
(3) edge of a knife of casting machine is heated to 50 DEG C, casting films glue is transferred to the storage tank of casting machine, by storage tank
It is heated to 50 DEG C, control edge of a knife slit width is 0.3mm, knife-band gap is 0.4mm, speed of service 2.6m/min, allows mixed solution
The curtain coating edge of a knife is flowed into start casting machine after full of the edge of a knife, smooth film is scraped on stainless steel band；
(4) by casting films obtained in step (3) under the transmission of stainless steel band, pass through drying oven, baking oven air blower
It opens, temperature setting is 150 DEG C, time 1h；
(5) it by the cooling 10min of casting films obtained in step (4), obtains with a thickness of 0.03mm, uniform, surface is smooth
Casting films, casting films are taken off from stainless steel band, produce continuous film with automatic coiling machine；
(6) microwave continuous composite dielectric film obtained in step (5) is cut into the thin slice of 1.1m × 1.3m；
(7) thin slice tow sides obtained in step (6) are subjected to plasma activation processing (state China GH-PM14), processing
Condition is gas ratio (N2: H2)=0.6, flow 1000mL/min, power 1800W, time 45min；
(8) by treated in step (7) thin slice, the PFA film of a 0.013mm is respectively placed in two sides up and down, as base
This unit overlaps 9, places electrolytic copper foil respectively in superimposed top layer and bottom, carries out in high temperature laminating machine (Burkle)
Vacuum pressing-combining, pressing condition are 390 DEG C and 70Kg/cm2Lower hot pressing 2h obtains microwave complex media plate.
Embodiment 4
According to each component content in 1 table of embodiment, microwave complex media plate is prepared, comprising the following steps:
(1) hydrolysising solvent is added in coupling agent Z-6124, stirs evenly, with BaTiO3Ball mill is added together, 80
DEG C ball mill in stir 2h；
(2) after being cooled to room temperature, by whole materials, the solvent in ball mill, (volume ratio of water and ethyl alcohol is 8:2), helps
Agent, polytetrafluoroethylene (PTFE) (PTFE) lotion, ethylene-tetrafluoroethylene copolymer (ETFE) are added in high shear agitation kettle, 80
DEG C 90min is stirred with the speed of 500r/min, vacuum defoamation mode is set, casting films glue is obtained；Wherein fluororesin modified dose
Bonding force can be improved, micro-ceramic powder is used for reinforcing filler, and for water lytic agent for cooperating coupling reaction, auxiliary agent is viscous for glue
Stability is spent, solvent is adjusted for gelatin viscosity；
(3) edge of a knife of casting machine is heated to 60 DEG C, casting films glue is transferred to the storage tank of casting machine, by storage tank
It is heated to 60 DEG C, control edge of a knife slit width is 0.4mm, knife-band gap is 0.4mm, speed of service 2.5m/min, allows mixed solution
The curtain coating edge of a knife is flowed into start casting machine after full of the edge of a knife, smooth film is scraped on stainless steel band；
(4) by casting films obtained in step (3) under the transmission of stainless steel band, pass through drying oven, baking oven air blower
It opens, temperature setting is 160 DEG C, time 2h；
(5) it by the cooling 30min of casting films obtained in step (4), obtains with a thickness of 0.05mm, uniform, surface is smooth
Casting films, casting films are taken off from stainless steel band, produce continuous film with automatic coiling machine；
(6) microwave continuous composite dielectric film obtained in step (5) is cut into the thin slice of 1.1m × 1.3m；
(7) thin slice tow sides obtained in step (6) are subjected to plasma activation processing (state China GH-PM14), processing
Condition is gas ratio (N2: H2)=0.7, flow 1100mL/min, power 2000W, time 60min；
(8) by treated in step (7) thin slice, the FEP film of a 0.013mm is respectively placed in two sides up and down, as base
This unit overlaps 7, places electrolytic copper foil respectively in superimposed top layer and bottom, carries out in high temperature laminating machine (Burkle)
Vacuum pressing-combining, pressing condition are 370 DEG C and 100Kg/cm2Lower hot pressing 5h obtains microwave complex media plate.
Embodiment 5
According to each component content in 1 table of embodiment, microwave complex media plate is prepared, comprising the following steps:
(1) hydrolysising solvent is added in coupling agent Z-6124, Z-6030, stirs evenly, with melt of si O2、Al2O3, golden red
Ball mill is added in stone TiO together, stirs 2h in 90 DEG C of ball mill；
(2) after being cooled to room temperature, by whole materials, the solvent in ball mill, (volume ratio of water and ethyl alcohol is 8:2), helps
Agent, polytetrafluoroethylene (PTFE) (PTFE) lotion, ethylene-tetrafluoroethylene copolymer (ETFE), perfluoroethylene-propylene (FEP) are added to high speed
In shear agitation kettle, 120min is stirred in 80 DEG C of speed with 500r/min, vacuum defoamation mode is set, casting films glue is obtained
Liquid；Wherein bonding force can be improved for fluororesin modified dose, micro-ceramic powder is used for reinforcing filler, and water lytic agent is for cooperating coupling
Reaction, auxiliary agent are used for gelatin viscosity stability, and solvent is adjusted for gelatin viscosity；
(3) edge of a knife of casting machine is heated to 90 DEG C, casting films glue is transferred to the storage tank of casting machine, by storage tank
It is heated to 90 DEG C, control edge of a knife slit width is 0.5mm, knife-band gap is 0.4mm, speed of service 2.0m/min, allows mixed solution
The curtain coating edge of a knife is flowed into start casting machine after full of the edge of a knife, smooth film is scraped on stainless steel band；
(4) by casting films obtained in step (3) under the transmission of stainless steel band, pass through drying oven, baking oven air blower
It opens, temperature setting is 170 DEG C, time 3h；
(5) it by the cooling 40min of casting films obtained in step (4), obtains with a thickness of 0.1mm, stream uniform, surface is smooth
Prolong film, casting films are taken off from stainless steel band, produces continuous film with automatic coiling machine；
(6) microwave continuous composite dielectric film obtained in step (5) is cut into the thin slice of 1.1m × 1.3m；
(7) thin slice tow sides obtained in step (6) are subjected to plasma activation processing (state China GH-PM14), processing
Condition is gas ratio (N2: H2)=0.8, flow 1200mL/min, power 2200W, time 70min；
(8) by treated in step (7), thin slice overlaps 3, places one respectively in superimposed top layer and bottom
Then the PTFE film of 0.013mm places electrolytic copper foil in upper layer and lower layer, vacuum pressure is carried out in high temperature laminating machine (Burkle)
It closes, pressing condition is 385 DEG C and 100Kg/cm2Lower hot pressing 5h obtains microwave complex media plate.
Embodiment 6
The microwave complex media plate and commercial product that prepare in embodiment 2- embodiment 5 are measured, measuring method are as follows:
According to IPC-TM-650 2.5.5.5 clamp micro-strip wire testing method test dielectric constant and dielectric loss, according to IPC-TM-650
2.4.41 the thermal linear expansion coefficient for measuring X, Y, Z axis measures the anti-stripping of microwave complex media plate according to IPC TM-650 2.4.8
Intensity.
Table 2 is microwave complex media plate test result in embodiment 2- embodiment 5:
By table 2, it can be concluded that, microwave complex media plate prepared by the present invention passes through dispersion of the ceramic powder in PTFE medium
Structural improvement PTFE insufficient rigidity is used for a long time the shortcomings that being easily deformed, while can use a variety of ceramic powders and compound to obtain
The microwave complex media plate of high, medium and low any dielectric constant.Compared with the external series of products of comparative example 1-3, in the present invention
Casting method technical maturity, equipment is simple, and operation is cheap, is processed compared with comparative example using customization, operates complicated rolling equipment,
Requirement to equipment and operation is substantially reduced, equipment manufacturing cost and maintenance cost reduction by 50%, making sheet production cycle shortening 30%, and
The properties of composite substrate are approximate, are a kind of low cost, the high performance microwave complex media board fabrication method haveing excellent performance.
The above is only the preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-described embodiment,
It is within the scope of the invention with present inventive concept without the various process programs of substantial differences.
Claims (10)
1. a kind of curtain coating preparation method of microwave complex media plate, it is characterised in that: the following steps are included:
(1) casting films glue is prepared；
(2) it is cast: the casting films glue prepared in step (1) is placed in casting machine, obtain casting films；
(3) transmission drying: casting films obtained in step (2) are dried by drying oven；
(4) it demoulds: after casting films obtained in step (3) are cooled to room temperature, obtaining microwave composite dielectric film；
(5) it post-processes: the microwave composite dielectric film obtained in step (4) is subjected to plasma activation processing；
(6) lamination matches: using treated in step (5) microwave composite dielectric film as basic unit, with fluorine resin film overlapping
Matching, is overlapped, places metal foil respectively in superimposed top layer and bottom, vacuum pressing-combining is carried out in high temperature laminating machine,
Obtain microwave complex media plate.
2. the curtain coating preparation method of microwave complex media plate according to claim 1, it is characterised in that: the casting films glue
Liquid is made of the raw material of following weight fraction: 100 parts of PTFE emulsion solid content, fluororesin modified dose 1~10 part, micro-ceramic
100~400 parts of powder, 0.1~4 part of surface modifier, 0.08~5 part of hydrolysising solvent, 0.5~15 part of auxiliary agent, solvent 50~100
Part.
3. the curtain coating preparation method of microwave complex media plate according to claim 2, it is characterised in that: the casting films glue
Liquid the preparation method comprises the following steps:
(a) pretreatment of raw material: coupling agent is pre-processed by hydrolysising solvent and is hydrolyzed, and after ceramic powder is added, is placed in ball mill；
(b) wet-mixing: the material in ball mill, solvent, auxiliary agent, PTFE emulsion, fluororesin modified dose of addition high shear are stirred
It mixes in kettle, is stirred under the conditions of 60-80 DEG C.
4. the curtain coating preparation method of microwave complex media plate according to claim 2, it is characterised in that: the hydrolysising solvent
For one of water, methylene chloride, ethyl alcohol, acetone, propylene glycol monomethyl ether, dimethylbenzene or a variety of compoundings.
5. the curtain coating preparation method of microwave complex media plate according to claim 2, it is characterised in that: the micron order pottery
Porcelain powder is SiO2、TiO2、Al2O3、CaTiO3、SrTiO3、BaTiO3, one of AlN, BN, SiC or a variety of compoundings.
6. the curtain coating preparation method of microwave complex media plate according to claim 1, it is characterised in that: the casting films glue
Liquid is made of the raw material of following weight fraction: 100 parts of PTFE emulsion solid content, fluororesin modified dose 1~10 part, micro-ceramic
100~400 parts of powder, 0.1~4 part of surface modifier, 0.08~5 part of hydrolysising solvent, 0.5~15 part of auxiliary agent, solvent 50~100
Part.
7. the curtain coating preparation method of microwave complex media plate according to claim 1, it is characterised in that: the plasma is living
The condition for changing processing is N2: H2=0.4~0.8, flow is 800mL/min~1200mL/min, and power is 1600W~2200W,
Handle 35min~70min.
8. the curtain coating preparation method of microwave complex media plate according to claim 1, it is characterised in that: the fluororesin is thin
Film is one of polytetrafluoroethylene (PTFE), perfluoroalkoxy resin, perfluoroethylene-propylene or a variety of compoundings.
9. the curtain coating preparation method of microwave complex media plate according to claim 1, it is characterised in that: in high temperature laminating machine
The middle condition for carrying out vacuum pressing-combining are as follows: 350~390 DEG C, 25~100Kg/cm22~10h of lower hot pressing.
10. microwave made from the curtain coating preparation method using microwave complex media plate of any of claims 1-9 is multiple
Close dielectric-slab.
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| CN111546718A (en) * | 2020-04-15 | 2020-08-18 | 中国电子科技集团公司第三十八研究所 | Preparation method of microwave composite dielectric plate and prepared microwave composite dielectric plate |
| CN114015092A (en) * | 2021-11-18 | 2022-02-08 | 佛山(华南)新材料研究院 | Preparation method and application of composite dielectric film |
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| CN110744839A (en) * | 2019-11-01 | 2020-02-04 | 中国电子科技集团公司第四十六研究所 | Process for preparing composite dielectric plate based on low dielectric constant turning film |
| CN111546718A (en) * | 2020-04-15 | 2020-08-18 | 中国电子科技集团公司第三十八研究所 | Preparation method of microwave composite dielectric plate and prepared microwave composite dielectric plate |
| CN114015092A (en) * | 2021-11-18 | 2022-02-08 | 佛山(华南)新材料研究院 | Preparation method and application of composite dielectric film |
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