CN103387704B - A kind of ceramic-polymer composite microwave material and methods for making and using same thereof - Google Patents
A kind of ceramic-polymer composite microwave material and methods for making and using same thereof Download PDFInfo
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- CN103387704B CN103387704B CN201310334947.1A CN201310334947A CN103387704B CN 103387704 B CN103387704 B CN 103387704B CN 201310334947 A CN201310334947 A CN 201310334947A CN 103387704 B CN103387704 B CN 103387704B
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Abstract
The invention belongs to microwave dielectric material and manufacture field, particularly a kind of ceramic-polymer composite microwave material and methods for making and using same thereof.This composite microwave material is by ceramic phase and polymer phase two phase composite, wherein polymer phase is as body material, microwave-medium ceramics is as packing material, by microwave-medium ceramics is formed microwave-medium ceramics phase with after lapping parcel, recharge in polymer phase and obtain, the volume content of described microwave-medium ceramics phase is 0 ~ 50%, and the volume content of polymer phase is 50 ~ 100%.The preparation method of this matrix material is: first adopt organism or coupling agent to carry out surface modification to ceramic powder, then after using a small amount of polymer wrapped, adopts extruding-out process processing.The specific inductivity of this matrix material under microwave frequency (about 10GHz) is 3-13, and dielectric loss is 0.0003-0.001, can be applicable to the microwave device such as microstrip antenna, microwave base plate.
Description
Technical field
The invention belongs to microwave dielectric material and manufacture field, particularly a kind of ceramic-polymer composite microwave material and methods for making and using same thereof.
Background technology
In recent years, along with the fast development of the technology such as mobile communication, wireless broadband network, satellite-navigation, the military main application fields becoming microwave technology of civilian replacement, miniaturization, high-performance, low cost become the main trend that microwave product develops.
The miniaturization of microwave device needs microwave dielectric material to have higher specific inductivity, high performance then needs microwave dielectric material to have low dielectric loss (i.e. high quality factor) with the sensitivity of the integrity and microwave device that ensure signal, usually wishes that spillage of material is lower than thousandth.Current low-loss microwave dielectric ceramic materials and resin material are used widely on the products such as microwave base plate, microwave antenna, wave filter, resonator, Ba Lun.Microwave ceramic material has the advantages such as higher specific inductivity (6-100), lower dielectric loss and temperature stability are good, but fragility is large, complete processing is complicated, is mainly used in making the high performance microwave component of small size (as antenna for mobile phone, satellite navigation aerial, dielectric filter, resonator etc.).The advantages such as microwave resin material (as tetrafluoroethylene, polyimide etc.) has good toughness, easy processing, microwave base plate, microstrip antenna are used widely, but its specific inductivity little (about 2-3), be unfavorable for the miniaturization of product.Ceramic-polymer Composite, the mechanical tenacity of electrical property good for microwave ceramics and polymkeric substance, workability can be combined, improve the over-all properties of matrix material, therefore exploitation easily processing, low-loss (being less than thousandth) the ceramic-polymer composite microwave medium material that specific inductivity can reach about 10 has larger practical application meaning, particularly in microwave antenna application aspect.
Current commercial Ceramic-polymer Composite mainly adopts tetrafluoroethylene as matrix, the pottery such as titanium dioxide, calcium titanate, trichroite is as filler, its specific inductivity is at about 3-10, and dielectric loss mostly exceedes thousandth, is mainly used in microwave base plate.Tetrafluoroethylene has lower dielectric loss (ten thousand/left and right, 10GHz), but processing temperature high (about 360 DEG C), fluidity of molten is poor, molded or the curing molding complete processing of usual employing cold stamping die, its processing and forming technology poor performance.High density polyethylene(HDPE) (HDPE), polypropylene (PP) and polystyrene (PS) lossy microwave little (under 10GHz frequency about 3/10000ths), processing temperature is lower, be particularly suitable for preparing low-loss Ceramic-polymer Composite mutually as polymeric matrix, mostly adopt traditional mechanical mixing preparation method at present.The people such as George at InternationalJournalofAppliedCeramicTechnology, Vol7, No.4(2010) on report and adopt traditional mechanical mixing preparation method, with Li
2mgSiO
4the Ceramic-polymer Composite that (specific inductivity is 5.1) is ceramic phase, high density polyethylene(HDPE) (HDPE) and polystyrene (PS) are polymer phase, when the volume content of its ceramic phase is 50%, the specific inductivity of matrix material is less than 5, dielectric loss is 0.02, and high dielectric loss can not meet the application requiring of microwave antenna etc.The people such as G.Subodh are at AppliedPhysicsLetters95, and 062903 (2009) upper report adopts traditional mechanical mixing preparation method, with the Sr of high-k
9ce
2ti
12o
36for the Ceramic-polymer Composite that ceramic phase, epoxy resin and high density polyethylene(HDPE) (HDPE) are polymer phase, when ceramic phase volume content is 40%, although the specific inductivity of matrix material under 10GHz frequency can reach 12, dielectric loss is higher than 0.004.Visible, adopt traditional mechanical mixing preparation method can not obtain high-k, the polyethylene of low dielectric loss, polystyrene-based Ceramic-polymer Composite.
Extrusion moulding is the most frequently used complete processing of producing low-costly and in high volume of thermoplastic resin, particularly conical double-screw is extruded, can under larger shearing stress effect, realizes fully contacting of filler and resin boundary surface, Homogeneous phase mixing, thus the performance greatly improving mixture.High density polyethylene(HDPE) (HDPE), polypropylene (PP) and polystyrene (PS) processing temperature lower (lower than 200 DEG C), fluidity of molten is good, is well suited for extrusion moulding.Adopt blending extrusion moulding process can obtain the Ceramic-polymer Composite of high compact density, high ceramic phase volume content, be expected to obtain the ceramic-polymer composite microwave material that high-k, low dielectric loss, processing characteristics are good.
The object of the invention is to overcome the existing low-k of ceramic-polymer composite microwave material and the shortcoming of high loss, with the stupalith of high-k be disperse phase, low-loss high density polyethylene(HDPE) (HDPE) and polystyrene (PS) for body material, adopt ceramic grain surface modification, the ceramic-polymer composite microwave medium material being applicable to the application such as microstrip antenna, microwave base plate that polymer wrapped, the preparation of blending extrusion technique have high dielectric constant (3-13), low lossy microwave (being less than thousandth).
Summary of the invention
Not enough for prior art, the invention provides a kind of ceramic-polymer composite microwave material and methods for making and using same thereof.
A kind of ceramic-polymer composite microwave material, this composite microwave material is by ceramic phase and polymer phase two phase composite, wherein polymer phase is as body material, microwave-medium ceramics is as packing material, by microwave-medium ceramics is formed microwave-medium ceramics phase with after lapping parcel, recharge in polymer phase and obtain, the volume content of described microwave-medium ceramics phase is 0 ~ 50%, and the volume content of polymer phase is 50 ~ 100%.
Described polymer phase adopts high density polyethylene(HDPE) (HDPE), polypropylene (PP) or polystyrene (PS).
Described microwave-medium ceramics adopts BaO-Re mutually
2o
3-TiO
2system microwave material, under 1 ~ 3GHz, its specific inductivity is between 80 ~ 100, and dielectric loss is 0.0002, and its each component molar per-cent is as follows:
Described Re
2o
3for Nd
2o
3, Sm
2o
3and La
2o
3in one or more.
Described lapping adopts the polymkeric substance dissolving in dimethylbenzene or acetone.
Described lapping adopts Low Density Polyethylene (LDPE) or polystyrene (PS).
A preparation method for ceramic-polymer composite microwave material, it first adopts organism or coupling agent to carry out surface modification to microwave-medium ceramics phase powder, then after using a small amount of lapping coated, adopt the processing of blending extrusion moulding process, concrete scheme is as follows:
After being sintered at 1250 ~ 1350 DEG C of temperature by microwave-medium ceramics phase powder, be crushed to the fine powder that particle diameter is not more than 10 μm, then add the coupling agent accounting for microwave-medium ceramics phase powder total mass 2%, grinding is mixed, is oldly not less than 24 hours; Lapping is dissolved in solvent, adds old good microwave-medium ceramics phase powder, under continuous stirring, dry;
Mixed with polymer phase in proportion by microwave-medium ceramics phase powder good for surface treatment, adopt twin screw extruder extruding pelletization namely to obtain required composite material granular, temperature when extruding is 180 DEG C, rotating speed 30rpm.
Described coupling agent is titanate ester or silicone based coupling agent.
An application method for ceramic-polymer composite microwave material, is by after hot-forming under 160 ~ 240 DEG C of temperature, 20 ~ 50MPa pressure for this ceramic-polymer composite microwave material granule, is processed into the microwave product of required different shape.
Described microwave product is microwave antenna, microwave base plate or Ba Lun.
Beneficial effect of the present invention is:
Adopt the specific inductivity of the ceramic-polymer composite microwave material prepared by the inventive method about 3 ~ 13, and continuously adjustabe, there is low lossy microwave (being less than thousandth), be easy to the advantage of producing quantitatively.
Embodiment
The invention provides a kind of ceramic-polymer composite microwave material and methods for making and using same thereof, below in conjunction with embodiment, the present invention will be further described.
Embodiment 1
Adopt K90 model ceramic powder (Ba-Nd-Ti system, specific inductivity 88 are called for short BNT), at 1280 DEG C of temperature after sintering, planetary ball mill 30 minutes, discharging is dried, and crosses 120 mesh sieves.Add the tetrabutyl titanate accounting for K90 model powder quality 2%, after ground and mixed, in sealing bag old 24 hours stand-by.
By commercial polystyrene (PS), use alcohol ultrasonic cleaning, dry.PS and old good BNT powder are weighed separately by weight 25:205.Load weighted PS is put into 150ml xylene solvent, at 80 DEG C of temperature after stirring and dissolving, then adds and weighed BNT powder in proportion, be warming up to 120 DEG C, Keep agitation, until xylene solvent Distillation recovery is complete.Obtained powder is pulverized, crosses 60 mesh sieve twice.The volume content of gained powder: PS is the volume content of 40%, BNT is 60%.
By commercial powdered high-density polyethylene (HDPE), use alcohol ultrasonic cleaning, dry.The BNT powder mixing prepared by required weight ratio and previous step, planetary ball mill 15 minutes, discharging is dried, and crosses 60 mesh sieve twice.
Under 180 DEG C of temperature, 30rpm rotating speed, adopt vertebra shape twin screw extruder to extrude, be namely made into PS and wrap up HDPE-BNT matrix material.Hot-forming under 220 DEG C of temperature, 200MPa pressure.Testing of materials performance is as follows:
Embodiment 2
Adopt K90 model powder (Ba-Nd-Ti system, specific inductivity 88 are called for short BNT), at 1280 DEG C of temperature after sintering, planetary ball mill 30 minutes, discharging is dried, and crosses 120 mesh sieves.Add the tetrabutyl titanate accounting for K90 model powder quality 2%, after ground and mixed, in sealing bag old 24 hours stand-by.
By commercial Low Density Polyethylene (LDPE), use alcohol ultrasonic cleaning, dry.LDPE and old good BNT powder are weighed separately by weight 1.5:100.Load weighted LDPE is put into xylene solvent, at 80 DEG C of temperature after stirring and dissolving, then adds and weighed BNT powder, be warming up to 120 DEG C, Keep agitation, until xylene solvent Distillation recovery is complete.Obtained powder is pulverized, crosses 60 mesh sieve twice.
By commercial powdered high-density polyethylene (HDPE), use alcohol ultrasonic cleaning, dry.The BNT powder mixing prepared by required weight ratio and previous step, planetary ball mill 15 minutes, discharging is dried, and crosses 60 mesh sieve twice.
Under 180 DEG C of temperature, 30rpm rotating speed, adopt vertebra shape twin screw extruder to extrude, be namely made into HDPE-BNT matrix material.Hot-forming under 220 DEG C of temperature, 200MPa pressure.Testing of materials performance is as follows:
Claims (5)
1. a ceramic-polymer composite microwave material, it is characterized in that: this composite microwave material is by ceramic phase and polymer phase two phase composite, wherein polymer phase is as body material, microwave-medium ceramics is as packing material, by microwave-medium ceramics is formed microwave-medium ceramics phase with after lapping parcel, recharge in polymer phase and obtain, the volume content of described microwave-medium ceramics phase is 0 ~ 50%, and the volume content of polymer phase is 50 ~ 100%;
Described polymer phase adopts high density polyethylene, polypropylene PP or polystyrene PS;
Described microwave-medium ceramics adopts BaO-Re mutually
2o
3-TiO
2system microwave material, under 1 ~ 3GHz, its specific inductivity is between 80 ~ 100, and dielectric loss is 0.0002, and its each component molar per-cent is as follows:
Described Re
2o
3for Nd
2o
3, Sm
2o
3and La
2o
3in one or more;
Described lapping adopts the polymkeric substance dissolving in dimethylbenzene or acetone.
2. the preparation method of a kind of ceramic-polymer composite microwave material as claimed in claim 1, it is characterized in that, first adopt coupling agent to carry out surface modification to microwave-medium ceramics phase powder, then after using lapping coated, adopt the processing of blending extrusion moulding process, concrete scheme is as follows:
After being sintered at 1250 ~ 1350 DEG C of temperature by microwave-medium ceramics phase powder, be crushed to the fine powder that particle diameter is not more than 10 μm, then add the coupling agent accounting for microwave-medium ceramics phase powder total mass 2%, grinding is mixed, is oldly not less than 24 hours; Lapping is dissolved in solvent, adds old good microwave-medium ceramics phase powder, under continuous stirring, dry;
Mixed with polymer phase in proportion by microwave-medium ceramics phase powder good for surface treatment, adopt twin screw extruder extruding pelletization namely to obtain required composite material granular, temperature when extruding is 180 DEG C, rotating speed 30rpm.
3. preparation method according to claim 2, is characterized in that: described coupling agent is titanate ester or silicone based coupling agent.
4. the application method of a kind of ceramic-polymer composite microwave material as claimed in claim 1, it is characterized in that: by this ceramic-polymer composite microwave material granule at 160 ~ 240 DEG C of temperature, hot-forming under 20 ~ 50MPa pressure after, be processed into the microwave product of required different shape.
5. application method according to claim 4, is characterized in that: described microwave product is microwave antenna, microwave base plate or Ba Lun.
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| CN109786953A (en) * | 2019-01-23 | 2019-05-21 | 曹丹旦 | A kind of microlayer polymeric composite wave dielectric chip and its application |
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| CN111334030A (en) * | 2020-03-09 | 2020-06-26 | 广东四维新材料有限公司 | 5G filter based on high-dielectric resin composite material and preparation method thereof |
| CN111253685A (en) * | 2020-03-09 | 2020-06-09 | 南京阜太新材料科技有限公司 | Low-dielectric-constant low-loss easily-electroplated plastic, and preparation method and application thereof |
| CN112968262A (en) * | 2021-02-24 | 2021-06-15 | 郴州功田电子陶瓷技术有限公司 | High-performance composite dielectric filter, material and preparation method |
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|---|---|---|---|---|
| CN1703463A (en) * | 2003-01-24 | 2005-11-30 | Tdk株式会社 | Composite dielectric material and substrate |
| CN102585444A (en) * | 2012-03-15 | 2012-07-18 | 深圳光启创新技术有限公司 | Composite material, dielectric substrate based on composite material and manufacturing method for composite material |
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| JPH0869712A (en) * | 1994-08-29 | 1996-03-12 | Kyocera Corp | Resin-ceramic composite material and wiring board for electronic parts using the composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1703463A (en) * | 2003-01-24 | 2005-11-30 | Tdk株式会社 | Composite dielectric material and substrate |
| CN102585444A (en) * | 2012-03-15 | 2012-07-18 | 深圳光启创新技术有限公司 | Composite material, dielectric substrate based on composite material and manufacturing method for composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109786953A (en) * | 2019-01-23 | 2019-05-21 | 曹丹旦 | A kind of microlayer polymeric composite wave dielectric chip and its application |
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