CN105399421B - A kind of substrate high-permittivity microwave medium ceramics and preparation method thereof - Google Patents

A kind of substrate high-permittivity microwave medium ceramics and preparation method thereof Download PDF

Info

Publication number
CN105399421B
CN105399421B CN201510844435.9A CN201510844435A CN105399421B CN 105399421 B CN105399421 B CN 105399421B CN 201510844435 A CN201510844435 A CN 201510844435A CN 105399421 B CN105399421 B CN 105399421B
Authority
CN
China
Prior art keywords
medium ceramics
preparation
microwave
substrate high
ball milling
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN201510844435.9A
Other languages
Chinese (zh)
Other versions
CN105399421A (en
Inventor
庞利霞
刘卫国
周迪
王欣
纪红芬
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xian Technological University
Original Assignee
Xian Technological University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Xian Technological University filed Critical Xian Technological University
Priority to CN201510844435.9A priority Critical patent/CN105399421B/en
Publication of CN105399421A publication Critical patent/CN105399421A/en
Application granted granted Critical
Publication of CN105399421B publication Critical patent/CN105399421B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/50—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
    • C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
    • C04B2235/3203—Lithium oxide or oxide-forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3213—Strontium oxides or oxide-forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/76—Crystal structural characteristics, e.g. symmetry
    • C04B2235/768—Perovskite structure ABO3
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Insulating Materials (AREA)

Abstract

The invention discloses a kind of substrate high-permittivity microwave medium ceramics and preparation method thereof, belong to electronic ceramics and its preparation field.The chemical composition of the microwave-medium ceramics is：(1‑x)(1‑y)SrO‑(1‑x)yCaO‑x/4Li2O‑x/4Pr2O3‑TiO2, wherein, 0.70≤x≤0.80；0≤y≤0.30.The present invention is prepared using the method for simple and effective solid phase reaction sintering, it is the formula for choosing proper ratio first, choose suitable initial oxide, it is well mixed by the various oxides of ball milling, preliminary reaction is carried out by pre-sintered process oxide, the particle size of reactant is refined by secondary ball milling, required ceramics sample is obtained finally by sintering process.Pass through such a simple and easy effective preparation method, the dielectric constant of obtained ceramics sample changes with composition between 122.4~148.4, Qf is distributed in 1,170GHz~2,160GHz, resonant frequency temperature easily regulates and controls (108ppm/ DEG C~+77ppm/ DEG C), 1350 DEG C of sintering temperature.

Description

A kind of substrate high-permittivity microwave medium ceramics and preparation method thereof
Technical field
The invention belongs to electronic ceramics and its preparation field, more particularly to a kind of substrate is made pottery with high-permittivity microwave medium Porcelain and preparation method thereof.
Background technology
Microwave-medium ceramics are a kind of new ceramic materials to grow up for nearly more than 20 years.It refers to be applied to As dielectric material and the pottery of one or more functions is completed in microwave frequency band (mainly 300MHz~300GHz frequency ranges) circuit Ceramic material, it is the critical material for manufacturing microwave dielectric filter resonator.This material is in recent decades with mobile logical The new function ceramic material for developing rapidly and growing up of letter cause, its outstanding feature are that dielectric constant is high, loss is low, humorous Vibration frequency temperature coefficient is small, and is used to that dielectric resonator, diectric antenna, duplexer, medium wave circuit, medium frequency stabilization is made The microwave components such as oscillator.At present, these devices have been widely used in micro multi-channel communication, microwave radio relay communication, have moved and lead to The various fields such as letter, satellite television broadcasting communication, scatter communication, military radar and satellite navigation and location system.Be benefited in recent years Fast development in fields such as mobile communication, space flight, military affairs, modern medicines, microwave dielectric ceramic materials are also increasingly by people Concern, just developed rapidly with surprising speed.
Microstrip antenna is a kind of antenna form succeeded in developing phase early 1970s.Microstrip antenna is due to structure letter The low and excellent electrical property of list, small volume, cost obtains a wide range of applications in ICBM SHF satellite terminal field, particularly in recent years just The popularization of formula navigation product (automotive avigraph, smart mobile phone etc.) is taken, more make it that the dosage of microstrip antenna is increasing.For a long time with Come, satellite navigation aerial is mainly ceramic substrate with medium substrate material.It can be shortened based on the low-loss material of high-k The cabling line length of antenna practical application, the volume for reducing GPS＆Wifi Combo antennas is realized, before antenna performance is not reduced Put, solve the problems, such as that the increasingly harsher day space of lines caused by mobile phone ID is to the limitation of day space of lines is inadequate.
In summary, find, prepare with research with high-k, low-loss, near-zero resonance frequency temperature coefficient (TCF=0ppm/ DEG C), low cost, the new high dielectric microwave media ceramic of environmental protection become the focus of people's current research with again Point.
The content of the invention
It is an object of the invention to provide a kind of substrate high-permittivity microwave medium ceramics and preparation method thereof, the pottery Ceramic material relative dielectric constant is high, and microwave property is good, and temperature coefficient of resonance frequency is adjustable, thing phase composition and preparation method letter It is single.
The present invention is to be achieved through the following technical solutions：
A kind of substrate high-permittivity microwave medium ceramics, the chemical composition of the microwave-medium ceramics are：(1-x)(1- y)SrO-(1-x)yCaO-x/4Li2O-x/4Pr2O3-TiO2, wherein, 0.70≤x≤0.80；0≤y≤0.30.
In the microwave-medium ceramics, based on Perovskite Phase, Sr, Ca, Li, Pr occupy A positions, and Ti occupies B positions.
The relative dielectric constant of the microwave-medium ceramics is 122.4~148.4, microwave qualities factor Qf=1,170GHz ~2,160GHz, temperature coefficient of resonance frequency are -108ppm/ DEG C~+77ppm/ DEG C.
The invention also discloses a kind of preparation method of substrate high-permittivity microwave medium ceramics, including following step Suddenly：
1) (1-x) (1-y) SrO- (1-x) yCaO-x/4Li is pressed2O-x/4Pr2O3-TiO2Mol ratio in formula, take strontium, calcium With the carbonate and praseodymium and titanyl compound of lithium, through once ball milling after mixing, then dry, sieve and be pressed into blocks, 4.5h is incubated at 1150 DEG C, obtains sample burning block；Wherein, 0.70≤x≤0.80,0≤y≤0.30；
2) through secondary ball milling, then drying, granulation, sieving after sample burning block is crushed, then by the particle pressure after sieving Type is made, 2h is sintered at 1350 DEG C into porcelain, obtains substrate high-permittivity microwave medium ceramics.
The carbonate of the strontium, calcium and lithium is respectively SrCO3、CaCO3And Li2CO3；Praseodymium and the titanyl compound difference For Pr6O11And TiO2。
Carrying out a ball milling and during secondary ball milling, time of each ball milling be 4h~5h, the temperature of drying is 100 DEG C~ 120℃。
Described sieving, step 1) were the screen cloth of 120 mesh, and step 2) is sieved to be double-deck：Cross the sieve of 60 mesh and 120 mesh Net.
Described granulation is to mix powder with the aqueous solution of polyvinyl alcohol, and micron-sized spheric granules is then made.
The sintering of described step 2) is the sintering under air atmosphere.
Described step 2) it is compressing be pressed into it is block or cylindric.
Compared with prior art, the present invention has technique effect beneficial below：
Substrate high-permittivity microwave medium ceramics disclosed by the invention, chemical composition are：(1-x)(1-y)SrO-(1- x)yCaO-x/4Li2O-x/4Pr2O3-TiO2, wherein, 0.70≤x≤0.80；0≤y≤0.30, it is sintered at 1350 DEG C. The present invention is You Guan theoretical with dielectric according to morphology, and based on Perovskite Phase, Sr, Ca, Li, Pr occupy A positions, Ti B positions are occupied, by adjusting its equivalent ionic radius in A, B position and ionic polarizability, high dielectric is realized in wider compositional range Constant and low-dielectric loss, temperature coefficient of resonance frequency can regulate and control within the specific limits, to reach microwave communication device to micro- The requirement of ripple medium substrate.By appropriate ceramic process, can be sintered out in air atmosphere densification and possess excellent micro- The new function ceramics of ripple dielectric properties, this kind of ceramics can be used as radio frequency multilayer ceramic capacitor, chip microwave-medium resonance The dielectric material such as device or wave filter, ceramic antenna, multi-chip module (MCM) uses.
The substrate of the present invention is had the characteristics that with high-dielectric constant microwave-medium ceramics material：Relative dielectric constant is adjustable (122.4~148.4), microwave property is good (Qf=1,170GHz~2,160GHz), temperature coefficient of resonance frequency nearly zero and easily Regulate and control (- 108ppm/ DEG C~+77ppm/ DEG C), chemical composition and preparation technology are simple.
Present invention employs the method for most simple and effective solid phase reaction sintering to prepare, and is to choose proper ratio first Formula, chooses suitable initial oxide, is well mixed by the various oxides of ball milling, is made by pre-sintered process Obtain oxide and carry out preliminary reaction, the particle size of reactant is refined by secondary ball milling, is obtained finally by sintering process Required ceramics sample.It is normal by such a simple and easy effective preparation method, the dielectric of obtained ceramics sample Number changes with composition between 122.4~148.4, and Qf is distributed in 1,170GHz~2,160GHz, and resonant frequency temperature is easily adjusted Control (- 108ppm/ DEG C~+77ppm/ DEG C), 1350 DEG C of sintering temperature.
Embodiment
With reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and It is not to limit.
Substrate disclosed by the invention is with the recipe formulation of high-dielectric constant microwave-medium ceramics material：(1-x)(1-y) SrO-(1-x)yCaO-x/4Li2O-x/4Pr2O3-TiO2, wherein 0.70≤x≤0.80,0≤y≤0.30.
Aforesaid substrate is with the specific preparation method of high-dielectric constant microwave-medium ceramics material：
By chemical raw material SrCO3、CaCO3、Li2CO3、Pr6O11And TiO2By formula formula：(1-x)(1-y)SrO-(1-x) yCaO-x/4Li2O-x/4Pr2O3-TiO2(wherein 0.70≤x≤0.80,0≤y≤0.30) dispensing, is sufficiently mixed ball milling 4~5 Individual hour, dry, sieve, briquetting after levigate, then through 1200 DEG C of pre-burnings, and be incubated 4.5 hours；
Block after pre-burning is subjected to secondary ball milling, is granulated after levigate drying, is sieved through 60 mesh and 120 eye mesh screens are double-deck；
Porcelain is compressing on demand, 2 hours are then sintered at 1350 DEG C into porcelain, you can obtain substrate with high dielectric Constant microwave dielectric ceramic materials.
Embodiment 1：
By the raw material SrCO of purity assay3、CaCO3、Li2CO3、Pr6O11And TiO2By formula (1-x) (1-y) SrO- (1- x)yCaO-x/4Li2O-x/4Pr2O3-TiO2After molar ratio in (wherein x=0.70, y=0), ball milling is sufficiently mixed (200 revs/min) 4 hours, then drying at 120 DEG C, cross sieve, the briquetting of 120 mesh, through 1200 DEG C of insulations under air atmosphere 4.5 hours, obtain sample burning block；
Then secondary ball milling is carried out after sample burning block is crushed again, Ball-milling Time is 5 hours, is made after being dried at 120 DEG C Grain (mixing powder with the aqueous solution of polyvinyl alcohol, micron-sized spheric granules is then made), it is double through 60 mesh and 120 eye mesh screens Layer sieving, you can obtain required porcelain；Porcelain is compressing on demand, 2h is then sintered under 1350 DEG C of air into porcelain, i.e., It can obtain substrate high-permittivity microwave medium ceramics and preparation method thereof material.
The performance of this group of ceramic material reaches following index：
Sinter porcelain in 1350 DEG C of air into, the dielectric properties ε under microwaver=148.4 (1.5GHz), quality factor q= 1100, Qf=1,650GHz, TCF=+77ppm/ DEG C of the temperature coefficient of resonance frequency (25 DEG C~85 DEG C) under microwave.
Embodiment 2：
By the raw material SrCO of purity assay3、CaCO3、Li2CO3、Pr6O11And TiO2By formula (1-x) (1-y) SrO- (1- x)yCaO-x/4Li2O-x/4Pr2O3-TiO2After molar ratio in (wherein x=0.75, y=0), ball milling is sufficiently mixed (200 revs/min) 4 hours, then drying at 120 DEG C, cross sieve, the briquetting of 120 mesh, through 1200 DEG C of insulations under air atmosphere 4.5 hours, obtain sample burning block；
Then secondary ball milling is carried out after sample burning block is crushed again, Ball-milling Time is 5 hours, is made after being dried at 120 DEG C Grain (mixing powder with the aqueous solution of polyvinyl alcohol, micron-sized spheric granules is then made), it is double through 60 mesh and 120 eye mesh screens Layer sieving, you can obtain required porcelain；Porcelain is compressing on demand, 2h is then sintered under 1350 DEG C of air into porcelain, i.e., It can obtain substrate high-permittivity microwave medium ceramics and preparation method thereof material.
The performance of this group of ceramic material reaches following index：
Sinter porcelain in 1350 DEG C of air into, the dielectric properties ε under microwaver=139.1 (1.55GHz), quality factor q= 71000, Qf=1,550GHz, TCF=+1.5ppm/ DEG C of the temperature coefficient of resonance frequency (25 DEG C~85 DEG C) under microwave.
Embodiment 3：
By the raw material SrCO of purity assay3、CaCO3、Li2CO3、Pr6O11And TiO2By formula (1-x) (1-y) SrO- (1- x)yCaO-x/4Li2O-x/4Pr2O3-TiO2After molar ratio in (wherein x=0.70, y=0.30), ball milling is sufficiently mixed (200 revs/min) 4 hours, then drying at 120 DEG C, cross sieve, the briquetting of 120 mesh, through 1200 DEG C of insulations under air atmosphere 4.5 hours, obtain sample burning block；
Then secondary ball milling is carried out after sample burning block is crushed again, Ball-milling Time is 5 hours, is made after being dried at 120 DEG C Grain (mixing powder with the aqueous solution of polyvinyl alcohol, micron-sized spheric granules is then made), it is double through 60 mesh and 120 eye mesh screens Layer sieving, you can obtain required porcelain；Porcelain is compressing on demand, 2h is then sintered under 1350 DEG C of air into porcelain, i.e., It can obtain substrate high-permittivity microwave medium ceramics and preparation method thereof material.
The performance of this group of ceramic material reaches following index：
Sinter porcelain in 1350 DEG C of air into, the dielectric properties ε under microwaver=137.6 (1.56GHz), quality factor q= 1385, Qf=2,160GHz, TCF=+41ppm/ DEG C of the temperature coefficient of resonance frequency (25 DEG C~85 DEG C) under microwave.
Embodiment 4：
By the raw material SrCO of purity assay3、CaCO3、Li2CO3、Pr6O11And TiO2By formula (1-x) (1-y) SrO- (1- x)yCaO-x/4Li2O-x/4Pr2O3-TiO2After molar ratio in (wherein x=0.80, y=0), ball milling is sufficiently mixed (200 revs/min) 4 hours, then drying at 120 DEG C, cross sieve, the briquetting of 120 mesh, through 1200 DEG C of insulations under air atmosphere 4.5 hours, obtain sample burning block；
Then secondary ball milling is carried out after sample burning block is crushed again, Ball-milling Time is 5 hours, is made after being dried at 120 DEG C Grain (mixing powder with the aqueous solution of polyvinyl alcohol, micron-sized spheric granules is then made), it is double through 60 mesh and 120 eye mesh screens Layer sieving, you can obtain required porcelain；Porcelain is compressing on demand, 2h is then sintered under 1350 DEG C of air into porcelain, i.e., It can obtain substrate high-permittivity microwave medium ceramics and preparation method thereof material.
The performance of this group of ceramic material reaches following index：
Sinter porcelain in 1350 DEG C of air into, the dielectric properties ε under microwaver=129.6 (1.68GHz), quality factor q= 845, Qf=1,420GHz, TCF=-84ppm/ DEG C of the temperature coefficient of resonance frequency (25 DEG C~85 DEG C) under microwave.
Embodiment 5：
By the raw material SrCO of purity assay3、CaCO3、Li2CO3、Pr6O11And TiO2By formula (1-x) (1-y) SrO- (1- x)yCaO-x/4Li2O-x/4Pr2O3-TiO2After molar ratio in (wherein x=0.73, y=0.30), ball milling is sufficiently mixed (200 revs/min) 4 hours, then drying at 120 DEG C, cross sieve, the briquetting of 120 mesh, through 1200 DEG C of insulations under air atmosphere 4.5 hours, obtain sample burning block；
Then secondary ball milling is carried out after sample burning block is crushed again, Ball-milling Time is 5 hours, is made after being dried at 120 DEG C Grain (mixing powder with the aqueous solution of polyvinyl alcohol, micron-sized spheric granules is then made), it is double through 60 mesh and 120 eye mesh screens Layer sieving, you can obtain required porcelain；Porcelain is compressing on demand, 2h is then sintered under 1350 DEG C of air into porcelain, i.e., It can obtain substrate high-permittivity microwave medium ceramics and preparation method thereof material.
The performance of this group of ceramic material reaches following index：
Sinter porcelain in 1350 DEG C of air into, the dielectric properties ε under microwaver=133.2 (1.66GHz), quality factor q= 1253, Qf=2,080GHz, TCF=-2.4ppm/ DEG C of the temperature coefficient of resonance frequency (25 DEG C~85 DEG C) under microwave.
Embodiment 6：
By the raw material SrCO of purity assay3、CaCO3、Li2CO3、Pr6O11And TiO2By formula (1-x) (1-y) SrO- (1- x)yCaO-x/4Li2O-x/4Pr2O3-TiO2After molar ratio in (wherein x=0.80, y=0.30), ball milling is sufficiently mixed (200 revs/min) 4 hours, then drying at 120 DEG C, cross sieve, the briquetting of 120 mesh, through 1200 DEG C of insulations under air atmosphere 4.5 hours, obtain sample burning block；
Then secondary ball milling is carried out after sample burning block is crushed again, Ball-milling Time is 5 hours, is made after being dried at 120 DEG C Grain (mixing powder with the aqueous solution of polyvinyl alcohol, micron-sized spheric granules is then made), it is double through 60 mesh and 120 eye mesh screens Layer sieving, you can obtain required porcelain；Porcelain is compressing on demand, 2h is then sintered under 1350 DEG C of air into porcelain, i.e., It can obtain substrate high-permittivity microwave medium ceramics and preparation method thereof material.
The performance of this group of ceramic material reaches following index：
Sinter porcelain in 1350 DEG C of air into, the dielectric properties ε under microwaver=122.4 (1.71GHz), quality factor q= 684, Qf=1,170GHz, TCF=-108ppm/ DEG C of the temperature coefficient of resonance frequency (25 DEG C~85 DEG C) under microwave.
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to is assert The embodiment of the present invention is only limitted to this, for general technical staff of the technical field of the invention, is not taking off On the premise of from present inventive concept, some simple deduction or replace can also be made, should all be considered as belonging to the present invention by institute Claims of submission determine scope of patent protection.

Claims (8)

1. a kind of substrate high-permittivity microwave medium ceramics, it is characterised in that the chemical composition of the microwave-medium ceramics is： (1-x)(1-y)SrO-(1-x)yCaO-x/4Li2O-x/4Pr2O3-TiO2, wherein, 0.70≤x≤0.80；0≤y≤0.30；
In the microwave-medium ceramics, based on Perovskite Phase, Sr, Ca, Li, Pr occupy A positions, and Ti occupies B positions；
The relative dielectric constant of the microwave-medium ceramics is 122.4~148.4, microwave qualities factor Qf=1,170GHz~2, 160GHz, temperature coefficient of resonance frequency are -108ppm/ DEG C~+77ppm/ DEG C.
2. the preparation method of the substrate high-permittivity microwave medium ceramics described in claim 1, it is characterised in that including with Lower step：
1) (1-x) (1-y) SrO- (1-x) yCaO-x/4Li is pressed2O-x/4Pr2O3-TiO2Mol ratio in formula, take strontium, calcium and lithium Carbonate and praseodymium and titanyl compound, through once ball milling after mixing, then dry, sieve and be pressed into blocks, 1150 4.5h is incubated at DEG C, obtains sample burning block；Wherein, 0.70≤x≤0.80,0≤y≤0.30；
2) through secondary ball milling, then drying, granulation, sieving after sample burning block is crushed, then the particle after sieving is pressed into Type, 2h is sintered at 1350 DEG C into porcelain, obtains substrate high-permittivity microwave medium ceramics.
3. the preparation method of substrate high-permittivity microwave medium ceramics according to claim 2, it is characterised in that institute The carbonate for stating strontium, calcium and lithium is respectively SrCO3、CaCO3And Li2CO3；The praseodymium and titanyl compound are respectively Pr6O11With TiO2。
4. the preparation method of substrate high-permittivity microwave medium ceramics according to claim 2, it is characterised in that When carrying out a ball milling and secondary ball milling, the time of each ball milling is 4h~5h, and the temperature of drying is 100 DEG C~120 DEG C.
5. the preparation method of substrate high-permittivity microwave medium ceramics according to claim 2, it is characterised in that institute The sieving stated, step 1) were the screen cloth of 120 mesh, and step 2) is sieved to be double-deck：Cross the screen cloth of 60 mesh and 120 mesh.
6. the preparation method of substrate high-permittivity microwave medium ceramics according to claim 2, it is characterised in that institute The granulation stated is to mix powder with the aqueous solution of polyvinyl alcohol, and micron-sized spheric granules is then made.
7. the preparation method of substrate high-permittivity microwave medium ceramics according to claim 2, it is characterised in that institute The sintering for the step 2) stated is the sintering under air atmosphere.
8. the preparation method of substrate high-permittivity microwave medium ceramics according to claim 2, it is characterised in that institute The step 2) stated it is compressing be pressed into it is block or cylindric.
CN201510844435.9A 2015-11-26 2015-11-26 A kind of substrate high-permittivity microwave medium ceramics and preparation method thereof Expired - Fee Related CN105399421B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510844435.9A CN105399421B (en) 2015-11-26 2015-11-26 A kind of substrate high-permittivity microwave medium ceramics and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510844435.9A CN105399421B (en) 2015-11-26 2015-11-26 A kind of substrate high-permittivity microwave medium ceramics and preparation method thereof

Publications (2)

Publication Number Publication Date
CN105399421A CN105399421A (en) 2016-03-16
CN105399421B true CN105399421B (en) 2018-02-09

Family

ID=55465231

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510844435.9A Expired - Fee Related CN105399421B (en) 2015-11-26 2015-11-26 A kind of substrate high-permittivity microwave medium ceramics and preparation method thereof

Country Status (1)

Country Link
CN (1) CN105399421B (en)

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103880415B (en) * 2014-02-25 2015-11-18 桂林电子科技大学 A kind of low-loss high dielectric Sr 1-x-y(Ca 0.6m 0.8/3) y(Na 0.5e 0.5) xtiO 3microwave ceramics and preparation method thereof

Also Published As

Publication number Publication date
CN105399421A (en) 2016-03-16

Similar Documents

Publication Publication Date Title
CN106587987B (en) The preparation method of C0G microwave dielectric material and preparation method and ceramic material
US9199882B2 (en) Scheelite microwave dielectric ceramic material and preparation method thereof
CN110282968A (en) A kind of microwave dielectric ceramic materials and preparation method thereof
CN103232243A (en) Vanadate microwave dielectric ceramic Ca1. 5M3V3O12 and preparation method thereof
CN104003722A (en) Ultralow-dielectric constant microwave dielectric ceramic Li3AlV2O8 capable of being sintered at low temperature and preparation method thereof
CN102249670A (en) Low temperature sintered microwave dielectric ceramic Li2Ba1-xSrxTi4O16 and preparation method thereof
CN107986774A (en) Low temperature sintering high-dielectric constant microwave-medium ceramics material and preparation method thereof
CN105254293A (en) Microwave dielectric ceramic material and preparation method thereof
CN103113103B (en) Low temperature sintered microwave dielectric ceramic BiZn2VO6 and preparation method thereof
CN109231967A (en) Bi2O3-B2O3Binary system microwave dielectric ceramic materials and preparation method thereof
CN103951425B (en) A kind of temperature-stable scheelite-type structure microwave-medium ceramics and preparation method thereof
CN106187107B (en) A kind of highly reliable A G characteristic microwave dielectric material and preparation method thereof
CN103553612A (en) Microwave dielectric ceramic Ba6W2V2O17 capable of being sintered at low temperature and preparation method thereof
CN103496981A (en) Low-temperature sintering temperature-stable microwave dielectric ceramic Bi14W2O27 and preparation method thereof
CN103044025A (en) Molybdenum-based low-temperature sintering temperature stable type microwave dielectric ceramic material and preparation method thereof
CN106007707B (en) Mg-Nb doped bismuth titanate microwave-medium ceramics and preparation method thereof
CN104177085A (en) Molybdenum-based temperature-stable microwave medium ceramic and preparation method thereof
CN103539444A (en) Low temperature sintering microwave dielectric ceramic Ca2Bi2O5 and preparation method thereof
CN105294103B (en) A kind of vanadium base temperature-stable microwave-medium ceramics and preparation method thereof
CN103435342A (en) Titanate microwave dielectric ceramic Ba2Ti5Zn(1-x)MgxO13 and preparation method thereof
CN103232244A (en) Low temperature sinterable vanadate microwave dielectric ceramic Ca0.5M4V3O12 and preparation method thereof
CN103524126B (en) Low-temperature sintering microwave dielectric ceramic CaBi2O4 and preparation method thereof
CN104944937A (en) ZnAl2O4/Li4Ti5O12 microwave dielectric ceramic material and preparation method thereof
CN105399420B (en) A kind of Ti bases high-permittivity microwave medium ceramics and preparation method thereof
CN105399421B (en) A kind of substrate high-permittivity microwave medium ceramics and preparation method thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20180209

Termination date: 20181126

CF01 Termination of patent right due to non-payment of annual fee