CN102350825A - Process for preparing fluorine-containing high polymer high frequency circuit board material by hydrothermal method - Google Patents
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Abstract
The invention relates to a process for preparing a fluorine-containing high polymer high frequency circuit board material by a hydrothermal method, which belongs to the high frequency circuit substrate material field. The method comprises the following steps: uniformly mixing a polytetrafluoroethylene emulsion (PTFE), a fluoroethylenepropylene emulsion (FEP) and a polyfluoroalkoxy emulsion (PFA), adding salts, then adding a molecule guiding agent and a molecular weight regulator, uniformly mixing, adding in a reaction vessel for performing hydrothermal reaction to complete high-molecular secondary polymerization, acquiring a substance of dielectric inorganic compound nanoparticles coated with high-molecular, filtering, washing, drying, removing end group, sintering, rolling, cladding copper to obtain the high frequency circuit board material with different dielectric constants finally. The prepared high frequency circuit board is capable of satisfying each basic index of the high frequency circuit board, and has the advantages of adjustable dielectric constant, low loss, good mechanical property and the like; the dielectric constant can be adjusted by the circuit board according to the generated dielectric inorganic compound content, the range of the dielectric constant is 2-35 which can satisfy the different requirements.
Description
Technical field
The present invention relates to the preparation method of high-frequency line sheet material path, particularly adopt the process of Hydrothermal Preparation fluorine-containing polymer high-frequency line sheet material path, belong to the high-frequency circuit board field of materials.
Background technology
The fluorine-containing polymer high-frequency circuit board is meant compound other material of fluorine-containing polymer, and like pottery, glass fabric, nonwoven, the high frequency of producing covers copper circuit board.
In the high-speed signal transmission lines of printed circuit board lead; Can be divided into two big types at present: one type is high-frequency signal transmission electronic product; This series products is relevant with wireless electromagnetic wave; It is the product that transmits signal with sine wave, like radar, radio and television, mobile phone, microwave communication and optical-fibre communications etc.; Another kind of is the electronic product of high-speed logic signal transmission class; This series products is with digital data transmission; Equally also relevant with the transmission of electromagnetic square wave, this series products begins to be mainly used in aspects such as computer, now has been generalized to rapidly on the electronic product of household electrical appliances and communication.The development of the communication technology and the information processing technology improves constantly its operating frequency.
Reach at a high speed and transmit, microwave high-frequency printed board baseplate material is being had clear and definite requirement aspect the electrical characteristic.Aspect the high speed transmission, realize transmitting the low-loss of signal, the low delay, must select the less baseplate material of dielectric constant and dielectric loss angle tangent for use, fluorine-containing polymer is exactly wherein a kind of.Fluorine-containing polymer has following characteristics: 1. dielectric constant (ε) and dielectric loss angle tangent (tan δ) minimum, dielectric constant (ε) are stable under high frequency; 2. good mechanical property; 3. hot property is high; 4. high with the metal adhesive strength; 5. chemical-resistance is good; 6. excellent in cushion effect.So the high frequency substrate material that fluorine-containing polymer is best suited for also is the maximum microwave high-frequency printed circuit board base board material of employing amount nowadays.
Through the development of nearly more than ten years, the fluorine-containing polymer high-frequency circuit board has got into the comparatively ripe research and development phase at present.The present all kinds of fluorine-containing polymer high-frequency circuit boards of U.S. Rogers company, its dielectric constant is about 2.Domestic R&D work mainly contains: the composite panel that is used for high-frequency circuit board of Hsinchu County, Taiwan Province Industrial Technology Research Institute; The method for producing printed circuit board for local region high frequency circuit by half-addition of Dongguan ShengYi Electronics Co., Ltd promptly has the zone of requirement to embed Rogers sheet material to high frequency characteristics on common sheet material.The fluorine-containing polymer high-frequency circuit board is the hard foundation stone of mechanics of communication of new generation and information processing technology revolution; And home products can't satisfy the high-frequency circuit needs at all; Import Rogers sheet material costs an arm and a leg, so it is significant to domestic mechanics of communication and information processing technology industry to research and develop fluorine-containing polymer high-frequency circuit board and novel preparation technology with independent intellectual property right.
Summary of the invention
The object of the present invention is to provide a kind of process of Hydrothermal Preparation fluorine-containing polymer high-frequency line sheet material path; This HF link plate can satisfy the requirement of microwave high-frequency printed board substrate fully; And its dielectric constant can be regulated according to the content of the inorganic compound that generates, and satisfies different high-frequency circuit demands.
The concrete technical scheme that the present invention adopts is following:
A kind of process of Hydrothermal Preparation fluorine-containing polymer high-frequency line sheet material path; It is characterized in that: it is with ptfe emulsion (PTFE); Perfluoroethylene-propylene emulsion (FEP); After tetrafluoroethene-perfluor n-propyl vinyl ether copolymer emulsion (PFA) mixes; Add salt earlier; Add molecular guide agent and molecular weight regulator again; Behind the mixing; Add and carry out hydro-thermal reaction completion macromolecule after polymerization in the agitated reactor; And obtain the material that macromolecule coats the dielectric inorganic compound nano-particle; Then through filtering; Washing; Dry; Remove end group; Sintering; Rolling; Cover copper, obtain the high-frequency line sheet material path of differing dielectric constant at last.
Said hydro-thermal reaction has experienced two processes, and the one, the macromolecule after polymerization generates the dielectric inorganic compound nano-particle simultaneously, and the 2nd, macromolecule coats the dielectric inorganic compound nano-particle that generates.
Said dielectric inorganic compound nano-particle mainly is zirconates, titanate, zirconium titanate or CaCu 3 Ti 4 O etc., and wherein the dielectric constant of CaCu 3 Ti 4 O (CCTO) can be up to more than 10000.
The concrete processing step of Hydrothermal Preparation fluorine-containing polymer high-frequency line sheet material path according to the invention is following:
A, with ptfe emulsion (PTFE), perfluoroethylene-propylene emulsion (FEP), tetrafluoroethene-perfluor n-propyl vinyl ether copolymer emulsion (PFA) according to 6 ~ 7:3 ~ 4:7 ~ 9 (w) mix mix well after; Add 5 ~ 35% (w) salt earlier; Add the molecular weight regulator of the molecular guide agent and 0 ~ 10% (w) of 0 ~ 10% (w) again, mixing obtains mixed emulsion.
The concentration of said ptfe emulsion (PTFE) is 50% (w), and the concentration of perfluoroethylene-propylene emulsion (FEP) is that the concentration of 50% (w), tetrafluoroethene-perfluor n-propyl vinyl ether copolymer emulsion (PFA) is 30% (w).
Described salts reaction thing is selected from the nitrate of calcium, magnesium, zirconium, strontium, barium, zinc or copper; The perhaps acetate of calcium, magnesium, zirconium, strontium or barium; Also or the sulfate of zinc or copper; Positive butyl titanate etc. also.
Said molecular guide agent is selected from diisopropylamine.
Said molecular weight regulator is selected from the different monooctyl ester of 3-mercaptopropionic acid (IOMP), modification mercaptan, isopropyl alcohol or alkyl hydrosulfide.
B, the mixed emulsion that steps A is made add agitated reactor, be warmed up to 180 ~ 250 ℃ with the heating rate of 0.5 ~ 1.5 ℃/min after, under the pressure of 2 ~ 8Mpa, reaction 2 ~ 48hour obtains the material that macromolecule coats the dielectric inorganic compound nano-particle.
C, the reacted product particle of filtration step B spend deionised water earlier 3 ~ 5 times, dry 2 ~ 5hour under 80 ~ 100 ℃ of environment of temperature again, and < logical ammonia is with the degraded end group in the ultraviolet light pipe of 200nm for the wavelength X of packing into then.
D, will through the product particle after step C handles behind 320 ~ 380 ℃ of following sintering 10 ~ 48hour, be positioned over immediately in the milling train and be rolled into the thick thin plate of 0.1 ~ 3mm at 200 ~ 280 ℃.
E, in vacuum, temperature is 300 ~ 365 ℃, pressure is under 20 ~ 50Mpa environment, electrolytic copper foil is mixed on thin plate single face or two sides process single or double copper-clad plate material.
Technical advantage of the present invention shows following 3 points:
The organic facies of A, fluorine-containing polymer high-frequency line sheet material path mainly contains three kinds; Wherein PTFE mainly provides dielectric properties; FEP mainly provides thermoplastic property, and PFA mainly provides thermoplasticity and mechanical performance, and can improve the adhesive property of whole fluorine-containing polymer high-frequency line sheet material path.
The dielectric constant of B, fluorine-containing polymer high-frequency line sheet material path can be regulated according to the content of the inorganic compound that generates, and satisfies different high-frequency circuit demands, especially the actual needs of alternating-current resistance reactance coupling.
C, the inorganic compound that is used for regulating dielectric constant can be selected more kind, are not subjected to the market supply and demand, many condition restriction such as chemical reaction.
The specific embodiment
Embodiment 1
A, with the perfluoroethylene-propylene emulsion (FEP) of the ptfe emulsion (PTFE) of 2.048L, 1.024L, the tetrafluoroethene of 3.926L-perfluor n-propyl vinyl ether copolymer emulsion (PFA) mix mix well after, add 897.4g zirconium nitrate Zr (NO earlier
3)
4With 434.4g calcium nitrate Ca (NO
3)
2, adding 80g diisopropylamine and 70g isopropyl alcohol again, mixing obtains mixed emulsion.
The concentration of said ptfe emulsion (PTFE) is 50% (w), and the concentration of perfluoroethylene-propylene emulsion (FEP) is that the concentration of 50% (w), tetrafluoroethene-perfluor n-propyl vinyl ether copolymer emulsion (PFA) is 30% (w).
B, the mixed emulsion that steps A is made add the 10L autoclave; Dress still ratio is 70.5%, be warmed up to 200 ℃ with the heating rate of 1 ℃/min after, under the pressure of 4Mpa; Reaction 48hour obtains the material that macromolecule coats the dielectric inorganic compound nano-particle.
C, the reacted product particle of filtration step B spend deionised water earlier 5 times, and dry 2hour under 100 ℃ of environment of temperature leads to ammonia with the degraded end group in the ultraviolet light pipe of the wavelength X=100nm that packs into then again.
D, will through the product particle after step C handles behind 350 ℃ of following sintering 36hour, be positioned over immediately in the milling train and be rolled into the thick thin plate of 1mm at 260 ℃.
E, in vacuum, temperature is 340 ℃, pressure is under the 30Mpa environment, electrolytic copper foil is mixed on thin plate single face or two sides process single or double copper-clad plate material.
Through test
1, calcium zirconate CaZrO in the product particle of step C
3Nano-particle content is 14.9% (w), and PTFE content is 32.1% (w), and FEP content is 16.1% (w), and PFA content is 36.9% (w).
2, step e copper coin dielectric material performance is: under the 1MHz, and ε
r=2.7, tan δ=3 * 10
-4Under the 10GHz, ε
r=2.8, tan δ=8 * 10
-4
Embodiment 2
A, with the perfluoroethylene-propylene emulsion (FEP) of the ptfe emulsion (PTFE) of 1.982L, 1.038L, the tetrafluoroethene of 3.980L-perfluor n-propyl vinyl ether copolymer emulsion (PFA) mix mix well after, add 1.1164kg barium nitrate Ba (NO earlier
3)
2With the positive butyl titanate C of 1.4538kg
16H
36O
4Ti adds 90g diisopropylamine and the different monooctyl ester of 80g 3-mercaptopropionic acid (IOMP) again, and mixing obtains mixed emulsion.
The concentration of said ptfe emulsion (PTFE) is 50% (w), and the concentration of perfluoroethylene-propylene emulsion (FEP) is that the concentration of 50% (w), tetrafluoroethene-perfluor n-propyl vinyl ether copolymer emulsion (PFA) is 30% (w).
B, the mixed emulsion that steps A is made add the 10L autoclave; Dress still ratio is 72.6%, be warmed up to 180 ℃ with the heating rate of 0.5 ℃/min after, under the pressure of 5Mpa; Reaction 36hour obtains the material that macromolecule coats the dielectric inorganic compound nano-particle.
C, the reacted product particle of filtration step B spend deionised water earlier 4 times, and dry 4hour under 90 ℃ of environment of temperature leads to ammonia with the degraded end group in the ultraviolet light pipe of the wavelength X=160nm that packs into then again.
D, will through the product particle after step C handles behind 345 ℃ of following sintering 24hour, be positioned over immediately in the milling train and be rolled into the thick thin plate of 0.5mm at 200 ℃.
E, in vacuum, temperature is 365 ℃, pressure is under the 20Mpa environment, electrolytic copper foil is mixed on thin plate single face or two sides process single or double copper-clad plate material.
Through test
1, the barium titanate nano granule content is 26.9% (w) in the product particle of step C, and PTFE content is 26.8% (w), and FEP content is 14% (w), and PFA content is 32.3% (w).
2, step e copper coin dielectric material performance is: under the 1MHz, and ε
r=6.1, tan δ=2 * 10
-3Under the 10GHz, ε
r=6.2, tan δ=6.7 * 10
-4
Embodiment 3
A, with the perfluoroethylene-propylene emulsion (FEP) of the ptfe emulsion (PTFE) of 1.920L, 1.047L, the tetrafluoroethene of 4.030L-perfluor n-propyl vinyl ether copolymer emulsion (PFA) mix mix well after, add 1.3802kg calcium nitrate Ca (NO earlier
3)
2, the positive butyl titanate C of 1.4305kg
16H
36O
4Ti and 1.418kg zirconium nitrate Zr (NO
3)
4, adding 100g diisopropylamine and 90g alkyl hydrosulfide again, mixing obtains mixed emulsion.
The concentration of said ptfe emulsion (PTFE) is 50% (w), and the concentration of perfluoroethylene-propylene emulsion (FEP) is that the concentration of 50% (w), tetrafluoroethene-perfluor n-propyl vinyl ether copolymer emulsion (PFA) is 30% (w).
B, the mixed emulsion that steps A is made add the 10L autoclave; Dress still ratio is 73.4%, be warmed up to 220 ℃ with the heating rate of 1.5 ℃/min after, under the pressure of 6.5Mpa; Reaction 24hour obtains the material that macromolecule coats the dielectric inorganic compound nano-particle.
C, the reacted product particle of filtration step B spend deionised water earlier 4 times, and dry 3hour under 95 ℃ of environment of temperature leads to ammonia with the degraded end group in the ultraviolet light pipe of the wavelength X=130nm that packs into then again.
D, will through the product particle after step C handles behind 380 ℃ of following sintering 24hour, be positioned over immediately in the milling train and be rolled into the thick thin plate of 1.5mm at 280 ℃.
E, in vacuum, temperature is 350 ℃, pressure is under the 35Mpa environment, electrolytic copper foil is mixed on thin plate single face or two sides process single or double copper-clad plate material.
Through test
1, zirconium calcium titanate CaTi in the product particle of step C
0.5Zr
0.5O
3Nano-particle content is 31.4% (w), and PTFE content is 24.4% (w), and FEP content is 13.5% (w), and PFA content is 30.7% (w).
2, step e copper coin dielectric material performance is: under the 1MHz, and ε
r=4.2, tan δ=3 * 10
-4Under the 10GHz, ε
r=4.3, tan δ=1.2 * 10
-3
Embodiment 4
A, with the perfluoroethylene-propylene emulsion (FEP) of the ptfe emulsion (PTFE) of 1.885L, 1.077L, the tetrafluoroethene of 4.038L-perfluor n-propyl vinyl ether copolymer emulsion (PFA) mix mix well after, add 322.2g calcium nitrate Ca (NO earlier
3)
2, 941.4g copper sulphate CuSO
4With the positive butyl titanate C of 677.6g
16H
36O
4Ti adds 100g diisopropylamine and 100g modification mercaptan again, and mixing obtains mixed emulsion.
The concentration of said ptfe emulsion (PTFE) is 50% (w), and the concentration of perfluoroethylene-propylene emulsion (FEP) is that the concentration of 50% (w), tetrafluoroethene-perfluor n-propyl vinyl ether copolymer emulsion (PFA) is 30% (w).
B, the mixed emulsion that steps A is made add the 10L autoclave; Dress still ratio is 73.1%, be warmed up to 160 ℃ with the heating rate of 1 ℃/min after, under the pressure of 6Mpa; Reaction 24hour obtains the material that macromolecule coats the dielectric inorganic compound nano-particle.
C, the reacted product particle of filtration step B spend deionised water earlier 3 times, and dry 2hour under 80 ℃ of environment of temperature leads to ammonia with the degraded end group in the ultraviolet light pipe of the wavelength X=180nm that packs into then again.
D, will through the product particle after step C handles behind 350 ℃ of following sintering 45hour, be positioned over immediately in the milling train and be rolled into the thick thin plate of 1mm at 250 ℃.
E, in vacuum, temperature is 345 ℃, pressure is under the 40Mpa environment, electrolytic copper foil is mixed on thin plate single face or two sides process single or double copper-clad plate material.
Through test
1, CaCu 3 Ti 4 O CCTO nano-particle content is 31.1% (w) in the product particle of step C, and PTFE content is 24.1% (w), and FEP content is 13.8% (w), and PFA content is 31% (w).
2, step e copper coin dielectric material performance is: under the 1MHz, and ε
r=13.2, tan δ=9 * 10
-4
Under the 10GHz, ε
r=13.3, tan δ=5 * 10
-3
Claims (8)
1. the process of a Hydrothermal Preparation fluorine-containing polymer high-frequency line sheet material path; It is characterized in that: it is with ptfe emulsion; The perfluoroethylene-propylene emulsion; After tetrafluoroethene-perfluor n-propyl vinyl ether copolymer emulsion mixes; Add salt earlier; Add molecular guide agent and molecular weight regulator again; Behind the mixing; Add and carry out hydro-thermal reaction completion macromolecule after polymerization in the agitated reactor; And obtain the material that macromolecule coats the dielectric inorganic compound nano-particle; Then through filtering; Washing; Dry; Remove end group; Sintering; Rolling; Cover copper, obtain the high-frequency line sheet material path of differing dielectric constant at last.
2. the process of Hydrothermal Preparation fluorine-containing polymer high-frequency line sheet material path according to claim 1 is characterized in that: concrete processing step is following:
A, with ptfe emulsion, perfluoroethylene-propylene emulsion, tetrafluoroethene-perfluor n-propyl vinyl ether copolymer emulsion according to the weight ratio of 6 ~ 7:3 ~ 4:7 ~ 9 mix mix well after; Add 5 ~ 35 wt% salts earlier; Add the molecular guide agent of 0 ~ 10 wt% and the molecular weight regulator of 0 ~ 10 wt% again, mixing obtains mixed emulsion;
B, the mixed emulsion that steps A is made add agitated reactor, be warmed up to 180 ℃ ~ 250 ℃ with the heating rate of 0.5 ~ 1.5 ℃/min after, under the pressure of 2 ~ 8Mpa, reaction 2 ~ 48hour obtains the material that macromolecule coats the dielectric inorganic compound nano-particle;
C, the reacted product particle of filtration step B spend deionised water earlier 3 ~ 5 times, dry 2 ~ 5hour under 80 ~ 100 ℃ of environment of temperature again, and < logical ammonia is with the degraded end group in the ultraviolet light pipe of 200nm for the wavelength X of packing into then;
D, will through the product particle after step C handles behind 320 ~ 380 ℃ of following sintering 10 ~ 48hour, be positioned over immediately in the milling train and be rolled into the thick thin plate of 0.1 ~ 3mm at 200 ~ 280 ℃;
E, in vacuum, temperature is 300 ~ 365 ℃, pressure is under 20 ~ 50Mpa environment, electrolytic copper foil is mixed on thin plate single face or two sides process single or double copper-clad plate material.
3. the process of Hydrothermal Preparation fluorine-containing polymer high-frequency line sheet material path according to claim 1 and 2; It is characterized in that: the concentration of said ptfe emulsion is 50wt%, and the concentration of perfluoroethylene-propylene emulsion is that the concentration of 50 wt%, tetrafluoroethene-perfluor n-propyl vinyl ether copolymer emulsion is 30 wt%.
4. the process of Hydrothermal Preparation fluorine-containing polymer high-frequency line sheet material path according to claim 1 and 2, it is characterized in that: said salt is selected from the nitrate of calcium, magnesium, zirconium, strontium, barium, zinc or copper; The perhaps acetate of calcium, magnesium, zirconium, strontium or barium; Also or the sulfate of zinc or copper; It can also be positive butyl titanate.
5. the process of Hydrothermal Preparation fluorine-containing polymer high-frequency line sheet material path according to claim 1 and 2 is characterized in that: said molecular guide agent is selected from diisopropylamine.
6. the process of Hydrothermal Preparation fluorine-containing polymer high-frequency line sheet material path according to claim 1 and 2 is characterized in that: said molecular weight regulator is selected from the different monooctyl ester of 3-mercaptopropionic acid, modification mercaptan, isopropyl alcohol or alkyl hydrosulfide.
7. the process of Hydrothermal Preparation fluorine-containing polymer high-frequency line sheet material path according to claim 1 and 2 is characterized in that: said dielectric inorganic compound nano-particle mainly is zirconates, titanate, zirconium titanate or CaCu 3 Ti 4 O.
8. the process of Hydrothermal Preparation fluorine-containing polymer high-frequency line sheet material path according to claim 7 is characterized in that: said dielectric inorganic compound DIELECTRIC CONSTANTS
rIn 30 ~ 10000 scopes, wherein the dielectric constant of CaCu 3 Ti 4 O is up to more than 10000.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107278037A (en) * | 2017-06-29 | 2017-10-20 | 安徽升鸿电子有限公司 | The copper-clad plate of 6.5≤Dk≤10 is made using turning hot pressing mode |
| CN107311517A (en) * | 2017-06-29 | 2017-11-03 | 安徽升鸿电子有限公司 | The method that Dk ＞ 10 copper-clad plate base material is made using turning mode |
| CN107382291A (en) * | 2017-06-22 | 2017-11-24 | 庐江县典扬电子材料有限公司 | The preparation method of the copper-clad plate base materials of 2.2≤Dk ＜ 6.5 |
| CN107509311A (en) * | 2017-06-29 | 2017-12-22 | 安徽升鸿电子有限公司 | The method that the copper-clad plate base material of 6.5≤Dk≤10 is made using turning mode |
| CN114644846A (en) * | 2020-12-17 | 2022-06-21 | 常熟三爱富中昊化工新材料有限公司 | Fluorine-containing polymer emulsion copper-clad plate and preparation method thereof |
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| CN107382291A (en) * | 2017-06-22 | 2017-11-24 | 庐江县典扬电子材料有限公司 | The preparation method of the copper-clad plate base materials of 2.2≤Dk ＜ 6.5 |
| CN107278037A (en) * | 2017-06-29 | 2017-10-20 | 安徽升鸿电子有限公司 | The copper-clad plate of 6.5≤Dk≤10 is made using turning hot pressing mode |
| CN107311517A (en) * | 2017-06-29 | 2017-11-03 | 安徽升鸿电子有限公司 | The method that Dk ＞ 10 copper-clad plate base material is made using turning mode |
| CN107509311A (en) * | 2017-06-29 | 2017-12-22 | 安徽升鸿电子有限公司 | The method that the copper-clad plate base material of 6.5≤Dk≤10 is made using turning mode |
| CN114644846A (en) * | 2020-12-17 | 2022-06-21 | 常熟三爱富中昊化工新材料有限公司 | Fluorine-containing polymer emulsion copper-clad plate and preparation method thereof |
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| CN102350825B (en) | 2014-03-26 |
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