CN105732031A - Nickel-doped Li3Mg2NbO6 ceramic material and preparation method thereof - Google Patents

Nickel-doped Li3Mg2NbO6 ceramic material and preparation method thereof Download PDF

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CN105732031A
CN105732031A CN201610033053.2A CN201610033053A CN105732031A CN 105732031 A CN105732031 A CN 105732031A CN 201610033053 A CN201610033053 A CN 201610033053A CN 105732031 A CN105732031 A CN 105732031A
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powder
nbo
ceramic material
nickel
mixing
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吴海涛
毕金鑫
杨长红
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University of Jinan
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Abstract

The invention discloses a nickel-doped Li3Mg2NbO6 ceramic material with improved microwave dielectric properties and a preparation method thereof. The composition is Li3(Mg[1-x]Nix)2NbO6, wherein 0<=x<=0.1. The preparation method comprises the following steps: proportioning Li2CO3, MgO, NiO and Nb2O5 according to the chemical formula, mixing, drying, screening, presintering, granulating, carrying out pressure molding and the like, and sintering at 1050-1100 DEG C, thereby obtaining the doped Li3Mg2NbO6 ceramic. The Ni<2+> is used for doping, thereby obviously lowering the preparation temperature on the premise of ensuring the original microwave dielectric properties to be stable. The dielectric constant is up to 14.57-16.50, the quality factor Q.f is up to 43,947-71,023 GHz, and the temperature coefficient of resonance frequency is -17.4 to -31.8 ppm/DEG C. The nickel-doped Li3Mg2NbO6 ceramic material has the advantages of simple preparation technique and environmental protection process, and has great application value in industry.

Description

The doping of a kind of nickel Li3Mg2NbO6 Ceramic material and preparation method
Technical field
The invention belongs to a kind of ceramic compound being characterized with composition, relate to a kind of nickel and adulterate to improve Li3Mg2NbO6Pottery of microwave dielectric property and preparation method thereof.
Background technology
Microwave-medium ceramics (MWDC) refers to complete as dielectric material a kind of pottery of microwave signal process in microwave frequency band circuit, is a kind of novel electric function ceramic.Along with the fast development of Internet technology, information capacity exponentially property increases, and applying frequency develops towards higher frequency range, and portable terminal and mobile communication develop further towards directions such as miniaturization, highly integrated and high stabilizabilities.Simultaneously, the devices such as dielectric resonator, wave filter, capacitor need further to be improved in terms of the acceptance of electromagnetic wave couples with transmission, energy with signal and screens frequency, this just proposes requirements at the higher level to the components and parts in microwave circuit, and exploitation miniaturization, high stable, cheap and highly integrated Novel microwave dielectric ceramic have become the focus place of current research and development.
Microwave-medium ceramics, as manufacturing the key component of microwave device, should meet following performance requirement: (1) relative dielectric constant εrHeight to be tried one's best, this can allow device more miniaturization；(2) temperature coefficient of resonance frequency τ f Device the most just can be made when working, to have preferable stability as close as 0；(3) quality factor qfValue wants height, the most just can have excellent selecting frequency characteristic.According to relative dielectric constant εrSize different from use frequency range, generally can will have been developed that and the microwave-medium ceramics developed be divided into ultralow dielectric microwave dielectric ceramic, low εrWith the microwave dielectric ceramic of high q-factor, medium εrWith the microwave dielectric ceramic of Q-value, high εrLow reactance-resistance ratio microwave dielectric ceramic 4 class.
In the recent period, Li-Mg-Nb-O system microwave-medium ceramics is because its excellent microwave dielectric property is by the extensive concern of scientific research personnel.Li3Mg2NbO6As the class in this system, there is suitable DIELECTRIC CONSTANT ε r (16.8), the temperature coefficient of resonance frequency τ of nearly zero f (-27.2ppm/ DEG C), and higher quality factor qf(79,643 GHz), has miniaturization, high stable, the advantage such as cheap and integrated, but its higher sintering temperature (1250 DEG C) is unfavorable for the application of microwave communication, it is impossible to adapt to the development trend of modern communications.
Summary of the invention
The purpose of the present invention, is for reducing Li3Mg2NbO6The sintering temperature of pottery, it is provided that a kind of with Li2CO3, MgO and Nb2O5For primary raw material, and to mix appropriate Ni2+, prepare the microwave-medium ceramics with excellent microwave dielectric property.Above-mentioned ceramic material is according to Li3(Mg1-xNix)2NbO6(x=0-0.1) chemical formula dispensing, twice batch mixing 20-24h, calcined temperature 950-1050 DEG C.Ceramic material dominant is Li mutually3Mg2NbO6, its dielectric constant range is 14.57 ~ 16.50, quality factor qfScope is 43,947-71,023 GHz, temperature coefficient of resonance frequency scope is-17.4 ~-31.8 ppm/ DEG C.
The present invention is achieved by following technical solution.
(1) batch mixing: purity is more than the material powder of 99.99% according to formula Li3(Mg1-xNix)2NbO6Chemical general formula carry out dispensing, by powder, zirconium oxide balls, dehydrated alcohol adds in mixing bottle, batch mixing 20-24 hour in batch mixer；Slurry after batch mixing is placed in drying baker drying；
(2) step (1) dried powders mixture loading crucible is placed in Muffle furnace, 950-1050 DEG C of pre-burning 4 hours, obtains pre-burning powder body;
(3) rerolling
By the powder after step (2) pre-burning, zirconium oxide balls, dehydrated alcohol adds mixing bottle again, batch mixing 20-24 hour in batch mixer；Slurry after batch mixing is placed in drying baker drying；
(4) pelletize, molding
The powder dried in (3) is added paraffin and carries out pelletize as binding agent, after crossing 80 mesh standard sieves, then be pressed into green compact with powder compressing machine with the pressure of 200MPa；
(5) binder removal
Green compact are placed in Muffle furnace, binder removal four hours at 500 DEG C, discharge paraffin component；
(6) sintering
By the green compact after binder removal in 1050 DEG C-1100 DEG C sintering, it is incubated 4 hours.
The invention has the beneficial effects as follows: the present invention uses price the cheapest ceramic alumina powder to be raw material.Preparation process stoichiometric proportion controls accurately, and technique is simple, reproducible；The microwave ceramic powder granule of synthesis is tiny, uniform, and synthesis temperature is relatively low, it is easy to sintering, it is possible to achieve sinters in 1100 DEG C, has good microwave dielectric property simultaneously, meet the needs of future microwave components and parts.
Accompanying drawing explanation
Fig. 1 is Li of the present invention3Mg2NbO6The each embodiment related process parameters of pottery and microwave dielectric property chart.
Fig. 2 is Li of the present invention3Mg2NbO6Section Example X-ray diffraction analysis figure.
Detailed description of the invention
With detailed description of the invention, the present invention is described in further detail below in conjunction with the accompanying drawings.
Embodiment 1 。
(1) batch mixing: according to Li3(Mg1-xNix)2NbO6(x=0.02) stoichiometric proportion of microwave-medium ceramics thing phase, uses precision balance to weigh the lithium carbonate (Li that purity is 99.99%2CO3) 8.4700g, magnesium oxide (MgO) 6.0363g, nickel oxide (NiO) 0.2306g and niobium pentaoxide (Nb2O5)20.3133g.Powder after weighing is poured in mixing bottle, and adds 40g dehydrated alcohol and 400g zirconium oxide balls.The most a diameter of 1cm and a diameter of 0.5cm abrading-ball example in mass ratio are that 2:1 loads；The mixing bottle of powder, abrading-ball and dehydrated alcohol is positioned on batch mixer batch mixing 24 hours continuously, and batch mixer rotating speed is 200 r/min；With coarse mesh, the slurry after batch mixing is separated with abrading-ball, will separate after slurry be placed in 70-90 DEG C at drying baker in dry.
(2) pre-burning: the powder after step (1) being dried is placed in Muffle furnace pre-burning 4 hours at 1000 DEG C, can obtain the Li after pre-burning3(Mg0.98Ni0.02)2NbO6Powder body.
(3) rerolling: by the powder after step (2) pre-burning and 400g zirconium oxide balls, 40g dehydrated alcohol adds mixing bottle again, batch mixing 24 hours in batch mixer, and batch mixer rotating speed is 200 r/min；With coarse mesh, the slurry after batch mixing is separated with abrading-ball, will separate after slurry be placed in 70-90 DEG C at drying baker in dry.
(4) pelletize, molding: the powder dried in step (3) is added the paraffin that mass percent is 8% and carries out pelletize as binding agent, after crossing 80 mesh standard sieves, then be pressed into green compact with powder compressing machine with the pressure of 200MPa.
(5) binder removal: green compact are placed in Muffle furnace, binder removal four hours at 500 DEG C, discharge paraffin component.
(6) sintering: using high temperature furnace with 5 DEG C/min of programming rate, can realize it for 4 hours in 1100 DEG C of insulations and sinter porcelain into, its dielectric constant is 14.995, quality factor qfIt is 5.92 × 104 GHz, temperature coefficient of resonance frequency is-19.8ppm/ DEG C.
Embodiment 2 。
(1) batch mixing: according to Li3(Mg1-xNix)2NbO6(x=0.04) stoichiometric proportion of microwave-medium ceramics thing phase, uses precision balance to weigh the lithium carbonate (Li that purity is 99.99%2CO3) 8.4405g, magnesium oxide (MgO) 5.8924g, nickel oxide (NiO) 0.4596g and niobium pentaoxide (Nb2O5)20.2423g.Powder after weighing is poured in mixing bottle, and adds 40g dehydrated alcohol and 400g zirconium oxide balls.The most a diameter of 1cm and a diameter of 0.5cm abrading-ball example in mass ratio are that 2:1 loads；The mixing bottle of powder, abrading-ball and dehydrated alcohol is positioned on batch mixer batch mixing 24 hours continuously, and batch mixer rotating speed is 200 r/min；With coarse mesh, the slurry after batch mixing is separated with abrading-ball, will separate after slurry be placed in 70-90 DEG C at drying baker in dry.
(2) pre-burning: the powder after step (1) being dried is placed in Muffle furnace pre-burning 4 hours at 1050 DEG C, can obtain the Li after pre-burning3(Mg0.96Ni0.04)2NbO6Powder body.
(3) rerolling: by the powder after step (2) pre-burning and 400g zirconium oxide balls, 40g dehydrated alcohol adds mixing bottle again, batch mixing 24 hours in batch mixer, and batch mixer rotating speed is 200 r/min；With coarse mesh, the slurry after batch mixing is separated with abrading-ball, will separate after slurry be placed in 70-90 DEG C at drying baker in dry.
(4) pelletize, molding: the powder dried in step (3) is added the paraffin that mass percent is 8% and carries out pelletize as binding agent, after crossing 80 mesh standard sieves, then be pressed into green compact with powder compressing machine with the pressure of 200MPa.
(5) binder removal: green compact are placed in Muffle furnace, binder removal four hours at 500 DEG C, discharge paraffin component.
(6) sintering: using high temperature furnace with 5 DEG C/min of programming rate, can realize it for 4 hours in 1050 DEG C of insulations and sinter porcelain into, its dielectric constant is 15.507, quality factor qfIt is 5.93 × 104 GHz, temperature coefficient of resonance frequency is-17.4ppm/ DEG C.
Embodiment 3 。
(1) batch mixing: according to Li3(Mg1-xNix)2NbO6(x=0.04) stoichiometric proportion of microwave-medium ceramics thing phase, uses precision balance to weigh the lithium carbonate (Li that purity is 99.99%2CO3) 8.4405g, magnesium oxide (MgO) 5.8924g, nickel oxide (NiO) 0.4596g and niobium pentaoxide (Nb2O5)20.2423g.Powder after weighing is poured in mixing bottle, and adds 40g dehydrated alcohol and 400g zirconium oxide balls.The most a diameter of 1cm and a diameter of 0.5cm abrading-ball example in mass ratio are that 2:1 loads；The mixing bottle of powder, abrading-ball and dehydrated alcohol is positioned on batch mixer batch mixing 24 hours continuously, and batch mixer rotating speed is 200 r/min；With coarse mesh, the slurry after batch mixing is separated with abrading-ball, will separate after slurry be placed in 70-90 DEG C at drying baker in dry.
(2) pre-burning: the powder after step (1) being dried is placed in Muffle furnace pre-burning 4 hours at 1000 DEG C, can obtain the Li after pre-burning3(Mg0.96Ni0.04)2NbO6Powder body.
(3) rerolling: by the powder after step (2) pre-burning and 400g zirconium oxide balls, 40g dehydrated alcohol adds mixing bottle again, batch mixing 24 hours in batch mixer, and batch mixer rotating speed is 200 r/min；With coarse mesh, the slurry after batch mixing is separated with abrading-ball, will separate after slurry be placed in 70-90 DEG C at drying baker in dry.
(4) pelletize, molding: the powder dried in step (3) is added the paraffin that mass percent is 8% and carries out pelletize as binding agent, after crossing 80 mesh standard sieves, then be pressed into green compact with powder compressing machine with the pressure of 200MPa.
(5) binder removal: green compact are placed in Muffle furnace, binder removal four hours at 500 DEG C, discharge paraffin component.
(6) sintering: using high temperature furnace with 5 DEG C/min of programming rate, can realize it for 4 hours in 1100 DEG C of insulations and sinter porcelain into, its dielectric constant is 15.601, quality factor qfIt is 5.19 × 104 GHz, temperature coefficient of resonance frequency is-19.8ppm/ DEG C.
Embodiment 4 。
(1) batch mixing: according to Li3(Mg1-xNix)2NbO6(x=0.06) stoichiometric proportion of microwave-medium ceramics thing phase, uses precision balance to weigh the lithium carbonate (Li that purity is 99.99%2CO3) 8.4111g, magnesium oxide (MgO) 5.7496g, nickel oxide (NiO) 0.6870g and niobium pentaoxide (Nb2O5)20.1719g.Powder after weighing is poured in mixing bottle, and adds 40g dehydrated alcohol and 400g zirconium oxide balls.The most a diameter of 1cm and a diameter of 0.5cm abrading-ball example in mass ratio are that 2:1 loads；The mixing bottle of powder, abrading-ball and dehydrated alcohol is positioned on batch mixer batch mixing 24 hours continuously, and batch mixer rotating speed is 200 r/min；With coarse mesh, the slurry after batch mixing is separated with abrading-ball, will separate after slurry be placed in 70-90 DEG C at drying baker in dry.
(2) pre-burning: the powder after step (1) being dried is placed in Muffle furnace pre-burning 4 hours at 950 DEG C, can obtain the Li after pre-burning3(Mg0.94Ni0.06)2NbO6Powder body.
(3) rerolling: by the powder after step (2) pre-burning and 400g zirconium oxide balls, 40g dehydrated alcohol adds mixing bottle again, batch mixing 24 hours in batch mixer, and batch mixer rotating speed is 200 r/min；With coarse mesh, the slurry after batch mixing is separated with abrading-ball, will separate after slurry be placed in 70-90 DEG C at drying baker in dry.
(4) pelletize, molding: the powder dried in step (3) is added the paraffin that mass percent is 8% and carries out pelletize as binding agent, after crossing 80 mesh standard sieves, then be pressed into green compact with powder compressing machine with the pressure of 200MPa.
(5) binder removal: green compact are placed in Muffle furnace, binder removal four hours at 500 DEG C, discharge paraffin component.
(6) sintering: using high temperature furnace with 5 DEG C/min of programming rate, can realize it for 4 hours in 1050 DEG C of insulations and sinter porcelain into, its dielectric constant is 14.571, quality factor qfIt is 6.83 × 104 GHz, temperature coefficient of resonance frequency is-20.6ppm/ DEG C.
Embodiment 5 。
(1) batch mixing: according to Li3(Mg1-xNix)2NbO6(x=0.06) stoichiometric proportion of microwave-medium ceramics thing phase, uses precision balance to weigh the lithium carbonate (Li that purity is 99.99%2CO3) 8.4111g, magnesium oxide (MgO) 5.7496g, nickel oxide (NiO) 0.6870g and niobium pentaoxide (Nb2O5)20.1719g.Powder after weighing is poured in mixing bottle, and adds 40g dehydrated alcohol and 400g zirconium oxide balls.The most a diameter of 1cm and a diameter of 0.5cm abrading-ball example in mass ratio are that 2:1 loads；The mixing bottle of powder, abrading-ball and dehydrated alcohol is positioned on batch mixer batch mixing 24 hours continuously, and batch mixer rotating speed is 200 r/min；With coarse mesh, the slurry after batch mixing is separated with abrading-ball, will separate after slurry be placed in 70-90 DEG C at drying baker in dry.
(2) pre-burning: the powder after step (1) being dried is placed in Muffle furnace pre-burning 4 hours at 1000 DEG C, can obtain the Li after pre-burning3(Mg0.94Ni0.06)2NbO6Powder body.
(3) rerolling: by the powder after step (2) pre-burning and 400g zirconium oxide balls, 40g dehydrated alcohol adds mixing bottle again, batch mixing 24 hours in batch mixer, and batch mixer rotating speed is 200 r/min；With coarse mesh, the slurry after batch mixing is separated with abrading-ball, will separate after slurry be placed in 70-90 DEG C at drying baker in dry.
(4) pelletize, molding: the powder dried in step (3) is added the paraffin that mass percent is 8% and carries out pelletize as binding agent, after crossing 80 mesh standard sieves, then be pressed into green compact with powder compressing machine with the pressure of 200MPa.
(5) binder removal: green compact are placed in Muffle furnace, binder removal four hours at 500 DEG C, discharge paraffin component.
(6) sintering: using high temperature furnace with 5 DEG C/min of programming rate, can realize it for 4 hours in 1100 DEG C of insulations and sinter porcelain into, its dielectric constant is 15.973, quality factor qfIt is 5.50 × 104 GHz, temperature coefficient of resonance frequency is-24.6ppm/ DEG C.
Embodiment 6 。
(1) batch mixing: according to Li3(Mg1-xNix)2NbO6(x=0.08) stoichiometric proportion of microwave-medium ceramics thing phase, uses precision balance to weigh the lithium carbonate (Li that purity is 99.99%2CO3) 8.3819g, magnesium oxide (MgO) 5.6078g, nickel oxide (NiO) 0.9128g and niobium pentaoxide (Nb2O5)20.1020g.Powder after weighing is poured in mixing bottle, and adds 40g dehydrated alcohol and 400g zirconium oxide balls.The most a diameter of 1cm and a diameter of 0.5cm abrading-ball example in mass ratio are that 2:1 loads；The mixing bottle of powder, abrading-ball and dehydrated alcohol is positioned on batch mixer batch mixing 24 hours continuously, and batch mixer rotating speed is 200 r/min；With coarse mesh, the slurry after batch mixing is separated with abrading-ball, will separate after slurry be placed in 70-90 DEG C at drying baker in dry.
(2) pre-burning: the powder after step (1) being dried is placed in Muffle furnace pre-burning 4 hours at 1050 DEG C, can obtain the Li after pre-burning3(Mg0.92Ni0.08)2NbO6Powder body.
(3) rerolling: by the powder after step (2) pre-burning and 400g zirconium oxide balls, 40g dehydrated alcohol adds mixing bottle again, batch mixing 24 hours in batch mixer, and batch mixer rotating speed is 200 r/min；With coarse mesh, the slurry after batch mixing is separated with abrading-ball, will separate after slurry be placed in 70-90 DEG C at drying baker in dry.
(4) pelletize, molding: the powder dried in step (3) is added the paraffin that mass percent is 8% and carries out pelletize as binding agent, after crossing 80 mesh standard sieves, then be pressed into green compact with powder compressing machine with the pressure of 200MPa.
(5) binder removal: green compact are placed in Muffle furnace, binder removal four hours at 500 DEG C, discharge paraffin component.
(6) sintering: using high temperature furnace with 5 DEG C/min of programming rate, can realize it for 4 hours in 1050 DEG C of insulations and sinter porcelain into, its dielectric constant is 16.501, quality factor qfIt is 6.02 × 104 GHz, temperature coefficient of resonance frequency is-21.3ppm/ DEG C.
Embodiment 7 。
(1) batch mixing: according to Li3(Mg1-xNix)2NbO6(x=0.08) stoichiometric proportion of microwave-medium ceramics thing phase, uses precision balance to weigh the lithium carbonate (Li that purity is 99.99%2CO3) 8.3819g, magnesium oxide (MgO) 5.6078g, nickel oxide (NiO) 0.9128g and niobium pentaoxide (Nb2O5)20.1020g.Powder after weighing is poured in mixing bottle, and adds 40g dehydrated alcohol and 400g zirconium oxide balls.The most a diameter of 1cm and a diameter of 0.5cm abrading-ball example in mass ratio are that 2:1 loads；The mixing bottle of powder, abrading-ball and dehydrated alcohol is positioned on batch mixer batch mixing 24 hours continuously, and batch mixer rotating speed is 200 r/min；With coarse mesh, the slurry after batch mixing is separated with abrading-ball, will separate after slurry be placed in 70-90 DEG C at drying baker in dry.
(2) pre-burning: the powder after step (1) being dried is placed in Muffle furnace pre-burning 4 hours at 1000 DEG C, can obtain the Li after pre-burning3(Mg0.92Ni0.08)2NbO6Powder body.
(3) rerolling: by the powder after step (2) pre-burning and 400g zirconium oxide balls, 40g dehydrated alcohol adds mixing bottle again, batch mixing 24 hours in batch mixer, and batch mixer rotating speed is 200 r/min；With coarse mesh, the slurry after batch mixing is separated with abrading-ball, will separate after slurry be placed in 70-90 DEG C at drying baker in dry.
(4) pelletize, molding: the powder dried in step (3) is added the paraffin that mass percent is 8% and carries out pelletize as binding agent, after crossing 80 mesh standard sieves, then be pressed into green compact with powder compressing machine with the pressure of 200MPa.
(5) binder removal: green compact are placed in Muffle furnace, binder removal four hours at 500 DEG C, discharge paraffin component.
(6) sintering: using high temperature furnace with 5 DEG C/min of programming rate, can realize it for 4 hours in 1100 DEG C of insulations and sinter porcelain into, its dielectric constant is 15.2213, quality factor qfIt is 7.10 × 104 GHz, temperature coefficient of resonance frequency is-25.7ppm/ DEG C.
Embodiment 8 。
(1) batch mixing: according to Li3(Mg1-xNix)2NbO6(x=0.10) stoichiometric proportion of microwave-medium ceramics thing phase, uses precision balance to weigh the lithium carbonate (Li that purity is 99.99%2CO3) 8.3530g, magnesium oxide (MgO) 5.4669g, nickel oxide (NiO) 1.1370g and niobium pentaoxide (Nb2O5)20.0325g.Powder after weighing is poured in mixing bottle, and adds 40g dehydrated alcohol and 400g zirconium oxide balls.The most a diameter of 1cm and a diameter of 0.5cm abrading-ball example in mass ratio are that 2:1 loads；The mixing bottle of powder, abrading-ball and dehydrated alcohol is positioned on batch mixer batch mixing 24 hours continuously, and batch mixer rotating speed is 200 r/min；With coarse mesh, the slurry after batch mixing is separated with abrading-ball, will separate after slurry be placed in 70-90 DEG C at drying baker in dry.
(2) pre-burning: the powder after step (1) being dried is placed in Muffle furnace pre-burning 4 hours at 1000 DEG C, can obtain the Li after pre-burning3(Mg0.9Ni0.1)2NbO6Powder body.
(3) rerolling: by the powder after step (2) pre-burning and 400g zirconium oxide balls, 40g dehydrated alcohol adds mixing bottle again, batch mixing 24 hours in batch mixer, and batch mixer rotating speed is 200 r/min；With coarse mesh, the slurry after batch mixing is separated with abrading-ball, will separate after slurry be placed in 70-90 DEG C at drying baker in dry.
(4) pelletize, molding: the powder dried in step (3) is added the paraffin that mass percent is 8% and carries out pelletize as binding agent, after crossing 80 mesh standard sieves, then be pressed into green compact with powder compressing machine with the pressure of 200MPa.
(5) binder removal: green compact are placed in Muffle furnace, binder removal four hours at 500 DEG C, discharge paraffin component.
(6) sintering: using high temperature furnace with 5 DEG C/min of programming rate, can realize it for 4 hours in 1100 DEG C of insulations and sinter porcelain into, its dielectric constant is 15.1200, quality factor qfIt is 4.39 × 104 GHz, temperature coefficient of resonance frequency is-31.8ppm/ DEG C.

Claims (8)

1. the Li of a nickel doping3Mg2NbO6Ceramic material, it is characterised in that the composition expression formula of this ceramic material is: Li3(Mg1-xNix)2NbO6, wherein 0≤x≤0.1.
The Li of a kind of nickel the most according to claim 1 doping3Mg2NbO6Ceramic material, it is characterised in that the relative dielectric constant ε of described ceramic material r =14.57 ~ 16.50, quality factor qf=43,947-71,023 GHz, temperature coefficient of resonance frequency τ f= -17.4~-31.8 ppm/℃。
3. the Li of a nickel doping3Mg2NbO6The preparation method of ceramic material, it is characterised in that comprise the following steps: (1) batch mixing: purity is more than the material powder of 99.99% according to formula Li3(Mg1-xNix)2NbO6Chemical general formula carry out dispensing, by powder, zirconium oxide balls, dehydrated alcohol adds in mixing bottle, batch mixing 20-24 hour in batch mixer；Slurry after batch mixing is placed in drying baker drying；(2) step (1) dried powders mixture loading crucible is placed in Muffle furnace, 950-1050 DEG C of pre-burning 4 hours, obtains pre-burning powder body;(3) powder after step (2) pre-burning, zirconium oxide balls, dehydrated alcohol are added mixing bottle by rerolling again, batch mixing 20-24 hour in batch mixer；Slurry after batch mixing is placed in drying baker drying；(4) powder dried in (3) is added paraffin and carries out pelletize as binding agent by pelletize, molding, after crossing 80 mesh standard sieves, then is pressed into green compact with powder compressing machine with the pressure of 200MPa；(5) green compact are placed in Muffle furnace by binder removal, binder removal four hours at 500 DEG C, discharge paraffin component；(6) sintering is by the green compact after binder removal in 1050 DEG C-1100 DEG C sintering, is incubated 4 hours.
The Li of a kind of nickel the most according to claim 3 doping3Mg2NbO6The preparation method of ceramic material, it is characterised in that described ceramic powder raw material is respectively Li2CO3, MgO, NiO and Nb2O5Powder body.
The Li of a kind of nickel the most according to claim 3 doping3Mg2NbO6The preparation method of ceramic material, it is characterised in that described step (1), the material of (3), abrading-ball, the mass ratio of dehydrated alcohol is 1:10:1；A diameter of 1cm and a diameter of 0.5cm mill ball quality ratio are 2:1, and batch mixer rotating speed is 200 r/min.
The Li of a kind of nickel the most according to claim 3 doping3Mg2NbO6The preparation method of ceramic material, it is characterised in that described step (1), the temperature that (3) dry is 70～90 DEG C.
The Li of a kind of nickel the most according to claim 3 doping3Mg2NbO6The preparation method of ceramic material, it is characterised in that the pelletize described in step (4) is that the sample powder body after being dried by ball milling carries out adding hot mixing with the paraffin that mass fraction is 8%, and heating mixing temperature is 55-65 DEG C, makes micron-sized spheroidal particle.
The Li of a kind of nickel the most according to claim 3 doping3Mg2NbO6The preparation method of ceramic material, it is characterised in that the cylindrical green body that step (5) obtains is sintered under 1050 DEG C of-1100 DEG C of air atmosphere by described step (6), programming rate is 5 DEG C/min, and temperature retention time is 4h.
CN201610033053.2A 2016-01-19 2016-01-19 Nickel-doped Li3Mg2NbO6 ceramic material and preparation method thereof Pending CN105732031A (en)

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CN112457010A (en) * 2020-12-02 2021-03-09 电子科技大学 Rock salt type reconstructed superlattice structure microwave dielectric ceramic material and preparation method thereof

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CN112250441A (en) * 2020-10-28 2021-01-22 烟台大学 Microwave dielectric ceramic with low sintering temperature and adjustable dielectric property
CN112457010A (en) * 2020-12-02 2021-03-09 电子科技大学 Rock salt type reconstructed superlattice structure microwave dielectric ceramic material and preparation method thereof
CN112457010B (en) * 2020-12-02 2022-03-29 电子科技大学 Rock salt type reconstructed superlattice structure microwave dielectric ceramic material and preparation method thereof

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