CN105859281B - A kind of low Jie's ceramics as low-loss microwave medium and preparation method - Google Patents

A kind of low Jie's ceramics as low-loss microwave medium and preparation method Download PDF

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CN105859281B
CN105859281B CN201610261666.1A CN201610261666A CN105859281B CN 105859281 B CN105859281 B CN 105859281B CN 201610261666 A CN201610261666 A CN 201610261666A CN 105859281 B CN105859281 B CN 105859281B
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吴海涛
毕金鑫
刘青青
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University of Jinan
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Abstract

The invention discloses a kind of low Jie's ceramics as low-loss microwave medium and preparation methods.Ceramic material is prepared using conventional solid technique, and main object is mutually Li2Ni3TiO6.Microwave dielectric ceramic materials of the present invention have the characteristics that：Ceramic dielectric constant εrIt is 11.73~12.96, quality factor q f is 0.92~1.01 × 104GHz, temperature coefficient of resonance frequency TfIt is 25.3~16.5ppm/ DEG C；Ceramic object phase composition is stablized, and preparation process is simple, and process environmental protection, manufacturing cost is relatively low, is a kind of rising microwave dielectric material.

Description

A kind of low Jie's ceramics as low-loss microwave medium and preparation method
Technical field
A kind of low Jie's ceramics as low-loss microwave medium and preparation method.
Background technology
Microwave-medium ceramics (MWDC) refer to completing microwave signal process as dielectric material in microwave frequency band circuit A kind of ceramics are a kind of novel electric function ceramics.With the fast development of Internet technology, exponentially property increases information capacity Long, applying frequency develop towards higher frequency range, portable terminal and mobile communication further towards minimize, it is highly integrated and The directions such as high stabilizability are developed.Meanwhile the devices such as dielectric resonator, filter, capacitor electromagnetic wave receiving and transmission, Energy needs further to be improved in terms of coupling and screening frequency with signal, this just proposes more the component in microwave circuit High request, exploitation miniaturization, high stable, cheap and highly integrated Novel microwave dielectric ceramic have become to be researched and developed now Where focus.
Key component of the microwave-medium ceramics as manufacture microwave device, should meet following performance requirement：(1) opposite to be situated between Electric constant εrHeight that will be as possible, this can allow device more to minimize；(2) temperature coefficient of resonance frequency τfIt will be as close as 0, there is preferable stability when can just device be made to work in this way；(3) quality factor q f values want high, can just there is excellent choosing in this way Frequency characteristic.
In the recent period, Li-Ni-B-O (B=Ti, Sn, Zr) system microwave-medium ceramics are because of its excellent low-k, low damage Consume the extensive concern of microwave dielectric property and lower sintering temperature by scientific research personnel.Li2Ni3TiO6As in the system One kind has many advantages, such as that object is mutually stablized, is of low cost, is conducive to the exploitation and application of microwave-medium ceramics.
Invention content
The present invention provides a kind of low Jie's low-loss Li2Ni3TiO6Microwave-medium ceramics and preparation method.Above-mentioned microwave is situated between Matter ceramics are prepared using conventional solid technique, and sintering temperature is 1150-1250 DEG C.The main object of ceramic material is mutually Li2Ni3TiO6, Its permittivity εrIt is 11.73~12.96, quality factor q f is 0.92~1.01 × 104GHz, temperature coefficient of resonance frequency τf It is -25.3~-16.5ppm/ DEG C.Above-mentioned ceramic material is according to Li2Ni3TiO6Chemical formula dispensing, twice batch mixing about for 24 hours, pre-burning temperature 1000-1050 DEG C of degree, 1150-1250 DEG C of sintering temperature, specific preparation process are as follows.
1. batch mixing：Purity is more than to 99.99% Li2CO3, NiO, TiO2Powder is according to formula Li2Ni3TiO6Chemical formula Dispensing is carried out, by powder, zirconium oxide balls, absolute ethyl alcohol is added in mixing bottle, abrading-ball in mixing process, the quality of absolute ethyl alcohol Ratio is 1:10:1；A diameter of 1cm and a diameter of 0.5cm mill ball qualities ratio are 2:1, batch mixer rotating speed is 200r/min, is mixed Expect about 24 hours time；It will be dried in drying box that slurry after batch mixing is placed at 70~90 DEG C.
2. powders mixture of the step (1) after dry is fitted into crucible to be placed in high temperature furnace, at 1000~1050 DEG C Pre-burning 4 hours, obtains pre-burning powder.
3. rerolling：By the powder after step (2) pre-burning, zirconium oxide balls, mixing bottle is added in absolute ethyl alcohol again, Batch mixing about 24 hours in batch mixer；Slurry after batch mixing is placed in 70~90 DEG C of drying box and is dried.
4. being granulated, molding：By powder addition mass percent dry in (3) for 8% paraffin as adhesive into Row is granulated, and heating mixing temperature is 55-65 DEG C, will be made after micron-sized spheric granules crosses 60-80 mesh standard sieves, then use powder Tablet press machine is pressed into cylindrical green body with the pressure of 200MPa.
5. dumping：Cylindrical green body is placed in high temperature furnace, the dumping four hours at about 500 DEG C, paraffin component is discharged.
6. sintering：By the cylindrical green body after dumping in 1150-1250 DEG C of sintering, 4 hours are kept the temperature, heating gradient is 5 DEG C /min。
The beneficial effects of the invention are as follows：The present invention uses the more cheap ceramic alumina powder of price for raw material.Prepare work The metering of skill process chemistry is more accurate than controlling, simple for process, reproducible；The Li of synthesis2Ni3TiO6Object mutually stablizes single, no dephasign Interference；The microwave ceramic powder particle of synthesis is tiny, uniform, and synthesis temperature is low, is easy to be sintered.Manufactured ceramics have low dielectric The low-loss microwave dielectric property of constant disclosure satisfy that the needs of future microwave component development.
Description of the drawings
Fig. 1 is Li of the present invention2Ni3TiO6Each embodiment related process parameters of ceramics and microwave dielectric property chart.
Fig. 2 is Li of the present invention2Ni3TiO6Ceramics sample X-ray diffraction analysis figure.
Invention is further described in detail with specific implementation mode below in conjunction with the accompanying drawings.
Specific implementation mode
Embodiment 1.
(1) batch mixing：According to Li2Ni3TiO6The stoichiometric ratio of microwave-medium ceramics object phase, is weighed pure using precision balance Lithium carbonate (the Li that degree is 99.99%2CO3) 3.69g, nickel oxide (NiO) 11.21g and titanium oxide (TiO2)3.99g.It will weigh Powder afterwards pours into mixing bottle, and 40g absolute ethyl alcohols and 400g zirconium oxide balls is added.Wherein a diameter of 1cm with it is a diameter of 0.5cm abrading-balls example in mass ratio is 2:1 is packed into；The mixing bottle of powder, abrading-ball and absolute ethyl alcohol is positioned on batch mixer continuously Batch mixing about 24 hours, batch mixer rotating speed are 200r/min；With coarse mesh by after batch mixing slurry and abrading-ball detach, after separation The drying box that is placed at 70-90 DEG C of slurry in dry.
(2) pre-burning：Powder after step (1) is dried is placed in Muffle furnace pre-burning 4 hours at 1050 DEG C, you can obtains Li after pre-burning2Ni3TiO6Powder.
(3) rerolling：By the powder and 400g zirconium oxide balls after step (2) pre-burning, 40g absolute ethyl alcohols are added again Mixing bottle, batch mixing about 24 hours in batch mixer, batch mixer rotating speed are 200r/min；With coarse mesh by the slurry and mill after batch mixing Ball detaches, and will be dried in drying box that the slurry after separation is placed at 70-90 DEG C.
(4) it is granulated, is molded：The paraffin for being 8% using the powder addition mass percent dried in step (3) is as bonding Agent is granulated, and after crossing 80 mesh standard sieves, then with powder compressing machine is pressed into cylindrical green body with the pressure of 200MPa.
(5) dumping：Cylindrical green body is placed in high temperature furnace, dumping four hours at 500 DEG C, paraffin component is discharged.
(6) it is sintered：It uses medium temperature Muffle furnace with 5 DEG C/min of heating rate, its sintering can be achieved within 4 hours in 1200 DEG C of heat preservations At porcelain, dielectric constant 12.31, quality factor q f is 1.01 × 104GHz, temperature coefficient of resonance frequency be- 17.4ppm/℃。
Specific implementation mode
Embodiment 2.
(1) batch mixing：According to Li2Ni3TiO6The stoichiometric ratio of microwave-medium ceramics object phase, is weighed pure using precision balance Lithium carbonate (the Li that degree is 99.99%2CO3) 3.69g, nickel oxide (NiO) 11.21g and titanium oxide (TiO2)3.99g.It will weigh Powder afterwards pours into mixing bottle, and 40g absolute ethyl alcohols and 400g zirconium oxide balls is added.Wherein a diameter of 1cm with it is a diameter of 0.5cm abrading-balls example in mass ratio is 2:1 is packed into；The mixing bottle of powder, abrading-ball and absolute ethyl alcohol is positioned on batch mixer continuously Batch mixing about 24 hours, batch mixer rotating speed are 200r/min；With coarse mesh by after batch mixing slurry and abrading-ball detach, after separation The drying box that is placed at 70-90 DEG C of slurry in dry.
(2) pre-burning：Powder after step (1) is dried is placed in Muffle furnace pre-burning 4 hours at 1000 DEG C, you can obtains Li after pre-burning2Ni3TiO6Powder.
(3) rerolling：By the powder and 400g zirconium oxide balls after step (2) pre-burning, 40g absolute ethyl alcohols are added again Mixing bottle, batch mixing about 24 hours in batch mixer, batch mixer rotating speed are 200r/min；With coarse mesh by the slurry and mill after batch mixing Ball detaches, and will be dried in drying box that the slurry after separation is placed at 70-90 DEG C.
(4) it is granulated, is molded：The paraffin for being 8% using the powder addition mass percent dried in step (3) is as bonding Agent is granulated, and after crossing 80 mesh standard sieves, then with powder compressing machine is pressed into cylindrical green body with the pressure of 200MPa.
(5) dumping：Cylindrical green body is placed in high temperature furnace, dumping four hours at 500 DEG C, paraffin component is discharged.
(6) it is sintered：It uses medium temperature Muffle furnace with 5 DEG C/min of heating rate, its sintering can be achieved within 4 hours in 1150 DEG C of heat preservations At porcelain, dielectric constant 11.73, quality factor q f is 0.93 × 104GHz, temperature coefficient of resonance frequency are -25.3 ppm/℃。
Embodiment 3.
(1) batch mixing：According to Li2Ni3TiO6The stoichiometric ratio of microwave-medium ceramics object phase, is weighed pure using precision balance Lithium carbonate (the Li that degree is 99.99%2CO3) 3.69g, nickel oxide (NiO) 11.21g and titanium oxide (TiO2)3.99g.It will weigh Powder afterwards pours into mixing bottle, and 40g absolute ethyl alcohols and 400g zirconium oxide balls is added.Wherein a diameter of 1cm with it is a diameter of 0.5cm abrading-balls example in mass ratio is 2:1 is packed into；The mixing bottle of powder, abrading-ball and absolute ethyl alcohol is positioned on batch mixer continuously Batch mixing about 24 hours, batch mixer rotating speed are 200r/min；With coarse mesh by after batch mixing slurry and abrading-ball detach, after separation The drying box that is placed at 70-90 DEG C of slurry in dry.
(2) pre-burning：Powder after step (1) is dried is placed in Muffle furnace pre-burning 4 hours at 1050 DEG C, you can obtains Li after pre-burning2Ni3TiO6Powder.
(3) rerolling：By the powder and 400g zirconium oxide balls after step (2) pre-burning, 40g absolute ethyl alcohols are added again Mixing bottle, batch mixing about 24 hours in batch mixer, batch mixer rotating speed are 200r/min；With coarse mesh by the slurry and mill after batch mixing Ball detaches, and will be dried in drying box that the slurry after separation is placed at 70-90 DEG C.
(4) it is granulated, is molded：The paraffin for being 8% using the powder addition mass percent dried in step (3) is as bonding Agent is granulated, and after crossing 80 mesh standard sieves, then with powder compressing machine is pressed into cylindrical green body with the pressure of 200MPa.
(5) dumping：Cylindrical green body is placed in high temperature furnace, dumping four hours at 500 DEG C, paraffin component is discharged.
(6) it is sintered：It uses medium temperature Muffle furnace with 5 DEG C/min of heating rate, its sintering can be achieved within 4 hours in 1250 DEG C of heat preservations At porcelain, dielectric constant 12.96, quality factor q f is 0.98 × 104GHz, temperature coefficient of resonance frequency are -21.7 ppm/℃。
Embodiment 4.
(1) batch mixing：According to Li2Ni3TiO6The stoichiometric ratio of microwave-medium ceramics object phase, is weighed pure using precision balance Lithium carbonate (the Li that degree is 99.99%2CO3) 3.69g, nickel oxide (NiO) 11.21g and titanium oxide (TiO2)3.99g.It will weigh Powder afterwards pours into mixing bottle, and 40g absolute ethyl alcohols and 400g zirconium oxide balls is added.Wherein a diameter of 1cm with it is a diameter of 0.5cm abrading-balls example in mass ratio is 2:1 is packed into；The mixing bottle of powder, abrading-ball and absolute ethyl alcohol is positioned on batch mixer continuously Batch mixing about 24 hours, batch mixer rotating speed are 200r/min；With coarse mesh by after batch mixing slurry and abrading-ball detach, after separation The drying box that is placed at 70-90 DEG C of slurry in dry.
(2) pre-burning：Powder after step (1) is dried is placed in Muffle furnace pre-burning 4 hours at 1000 DEG C, you can obtains Li after pre-burning2Ni3TiO6Powder.
(3) rerolling：By the powder and 400g zirconium oxide balls after step (2) pre-burning, 40g absolute ethyl alcohols are added again Mixing bottle, batch mixing about 24 hours in batch mixer, batch mixer rotating speed are 200r/min；With coarse mesh by the slurry and mill after batch mixing Ball detaches, and will be dried in drying box that the slurry after separation is placed at 70-90 DEG C.
(4) it is granulated, is molded：The paraffin for being 8% using the powder addition mass percent dried in step (3) is as bonding Agent is granulated, and after crossing 80 mesh standard sieves, then with powder compressing machine is pressed into cylindrical green body with the pressure of 200MPa.
(5) dumping：Cylindrical green body is placed in high temperature furnace, dumping four hours at 500 DEG C, paraffin component is discharged.
(6) it is sintered：It uses medium temperature Muffle furnace with 5 DEG C/min of heating rate, its sintering can be achieved within 4 hours in 1250 DEG C of heat preservations At porcelain, dielectric constant 12.78, quality factor q f is 0.92 × 104GHz, temperature coefficient of resonance frequency are -23.3 ppm/℃。
Embodiment 5.
(1) batch mixing：According to Li2Ni3TiO6The stoichiometric ratio of microwave-medium ceramics object phase, is weighed pure using precision balance Lithium carbonate (the Li that degree is 99.99%2CO3) 3.69g, nickel oxide (NiO) 11.21g and titanium oxide (TiO2)3.99g.It will weigh Powder afterwards pours into mixing bottle, and 40g absolute ethyl alcohols and 400g zirconium oxide balls is added.Wherein a diameter of 1cm with it is a diameter of 0.5cm abrading-balls example in mass ratio is 2:1 is packed into；The mixing bottle of powder, abrading-ball and absolute ethyl alcohol is positioned on batch mixer continuously Batch mixing about 24 hours, batch mixer rotating speed are 200r/min；With coarse mesh by after batch mixing slurry and abrading-ball detach, after separation The drying box that is placed at 70-90 DEG C of slurry in dry.
(2) pre-burning：Powder after step (1) is dried is placed in Muffle furnace pre-burning 4 hours at 1050 DEG C, you can obtains Li after pre-burning2Ni3TiO6Powder.
(3) rerolling：By the powder and 400g zirconium oxide balls after step (2) pre-burning, 40g absolute ethyl alcohols are added again Mixing bottle, batch mixing about 24 hours in batch mixer, batch mixer rotating speed are 200r/min；With coarse mesh by the slurry and mill after batch mixing Ball detaches, and will be dried in drying box that the slurry after separation is placed at 70-90 DEG C.
(4) it is granulated, is molded：The paraffin for being 8% using the powder addition mass percent dried in step (3) is as bonding Agent is granulated, and after crossing 80 mesh standard sieves, then with powder compressing machine is pressed into cylindrical green body with the pressure of 200MPa.
(5) dumping：Cylindrical green body is placed in high temperature furnace, dumping four hours at 500 DEG C, paraffin component is discharged.
(6) it is sintered：It uses medium temperature Muffle furnace with 5 DEG C/min of heating rate, its sintering can be achieved within 4 hours in 1150 DEG C of heat preservations At porcelain, dielectric constant 11.93, quality factor q f is 0.98 × 104GHz, temperature coefficient of resonance frequency are -16.5 ppm/℃。

Claims (4)

1. a kind of low Jie's ceramics as low-loss microwave medium, it is characterised in that：The main object of ceramic material is mutually Li2Ni3TiO6, Permittivity ε after being sintered at 1150~1250 DEG CrIt is 11.73~12.96, quality factor q f is 0.92~1.01 × 104GHz, Temperature coefficient of resonance frequency τfIt is -25.3~-16.5ppm/ DEG C.
2. a kind of preparation method of low Jie's ceramics as low-loss microwave medium as described in claim 1, is made of following step：
(1) batch mixing：Purity is more than to 99.99% Li2CO3, NiO, TiO2Powder is according to formula Li2Ni3TiO6Chemical formula into Row dispensing, by powder, zirconium oxide balls, absolute ethyl alcohol is added in mixing bottle, batch mixing about 24 hours in batch mixer；After batch mixing The drying box that is placed at 70~90 DEG C of slurry in dry；
(2) pre-burning：Powders mixture of the step (1) after dry is fitted into crucible to be placed in high temperature furnace, at 1000~1050 DEG C Lower pre-burning 4 hours, obtains pre-burning powder；
(3) rerolling：By the powder after step (2) pre-burning, zirconium oxide balls, mixing bottle is added in absolute ethyl alcohol again, mixed Batch mixing about 24 hours in material machine；Slurry after batch mixing is placed in 70~90 DEG C of drying box and is dried；
(4) it is granulated, is molded：Using powder addition mass percent dry in step (3) for 8% paraffin as adhesive into Row is granulated, and after crossing 60-80 mesh standard sieves, then with powder compressing machine is pressed into green compact with the pressure of 200MPa；
(5) dumping：Green compact are placed in high temperature furnace, the dumping four hours at about 500 DEG C, paraffin component is discharged；
(6) it is sintered：By the green compact after dumping in 1150-1250 DEG C of sintering, 4 hours are kept the temperature.
3. a kind of preparation method of low Jie's ceramics as low-loss microwave medium according to claim 2, which is characterized in that the step (1), the mass ratio of the material of (3), abrading-ball, absolute ethyl alcohol is 1:10:1；A diameter of 1cm and a diameter of 0.5cm mill ball qualities ratio Example is 2:1, batch mixer rotating speed is 200r/min.
4. a kind of preparation method of low Jie's ceramics as low-loss microwave medium according to claim 2, which is characterized in that the step (6) cylindrical green body for obtaining step (5) is sintered 4 hours at 1150-1250 DEG C, and heating gradient is 5 DEG C/min.
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CN109111224A (en) * 2017-06-23 2019-01-01 天津大学 A kind of high-temperature stability lithium NiTi series microwave dielectric ceramic and its preparation method and application
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