CN109111226A - NaCa2Mg2V3O12The preparation method of microwave dielectric ceramic - Google Patents

NaCa2Mg2V3O12The preparation method of microwave dielectric ceramic Download PDF

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CN109111226A
CN109111226A CN201811111699.3A CN201811111699A CN109111226A CN 109111226 A CN109111226 A CN 109111226A CN 201811111699 A CN201811111699 A CN 201811111699A CN 109111226 A CN109111226 A CN 109111226A
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naca
dielectric ceramic
microwave dielectric
microwave
mixed powder
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周焕福
孙文东
刘晓斌
陈秀丽
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Guilin University of Technology
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Guilin University of Technology
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    • 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
    • C04B35/495—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 vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
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    • 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
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    • 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
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    • 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
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    • 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
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    • 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

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  • Inorganic Insulating Materials (AREA)

Abstract

The invention discloses a kind of NaCa2Mg2V3O12The preparation method of microwave dielectric ceramic.By NaCa2Mg2V3O12Stoichiometric ratio ingredient, it then is that 1:2:1 sequentially adds zirconia ball and dehydrated alcohol into mixed powder according to mixed powder, zirconia ball and dehydrated alcohol mass ratio, ball milling 4 hours, then it is dried at 100 ~ 120 DEG C, powder after drying is handled with the sieve sieving of 200 mesh, then being directly compressed into diameter is 12mm, the cylindric sample with a thickness of 6mm；Then sample is warming up to 775 ~ 875 DEG C with the heating rate of 5 DEG C/min, and the temperature is kept to be sintered 4 hours, obtain NaCa2Mg2V3O12Microwave dielectric ceramic.For the method for the present invention compared to traditional solid reaction process, successfully preparing in the case where saving the series of steps such as pre-burning, secondary ball milling, granulation and dumping has fine and close microstructure, higherQ×fValue and nearly zero τ f The microwave-medium ceramics of value.It ensure that the performance of material while further reducing the cost, simplifying experimental implementation, there is certain application potential.

Description

NaCa2Mg2V3O12The preparation method of microwave dielectric ceramic
Technical field
The invention belongs to electronic ceramics and its manufacturing field, in particular to a kind of NaCa2Mg2V3O12Microwave dielectric ceramic Preparation method.Resonator, filter, diectric antenna, the medium that the microwave dielectric ceramic can be used in using in microwave frequency band are led The microwave devices dielectric ceramic material such as wave circuit.
Background technique
Microwave dielectric material, which refers to, medium and completes one kind applied to being used as in microwave frequency band (300MHz ~ 300GHz) circuit Or the ceramics of multiple functions, mainly for the preparation of microwave devices such as resonator, filter, diectric antenna, dielectric guided wave circuits. In recent years, as microwave device is constantly to cost effective, miniaturization and the development in lightweight direction, it is desirable that microwave-medium material Material has excellent microwave dielectric property (sintering temperature and low, heightQ×fValue, low-k and nearly zeroτ f Value), low life Cost is produced to guarantee the transmission speed and temperature stability of signal.In recent years, many vanadium base microwave medium ceramic materials obtain Extensive research, such as Mg2V207, R2V2O7(R=Ba, Sr, Ca) and Ca5A4(VO4)6 (A2+=Mg, Zn), these ceramics are not only It with good microwave property, and can be sintered at low temperature, but preparation cost is higher, experimental procedure is cumbersome limits it Application commercially.Therefore, find low cost, reaction sintering easy to operate prepare vanadium base microwave medium ceramic material with Reducing cost can yet be regarded as a kind of new selection.Compared to traditional solid reaction process, reaction sintering is saving pre-burning, secondary ball Mill, be granulated and the series of steps such as dumping in the case where successfully prepare there is fine and close microstructure, higherQ×fIt is worth and close Zero τ f The microwave-medium ceramics of value.
NaCa2Mg2V3O12Ceramics have excellent microwave dielectric property (Q×f=25,924 GHz, ε r =7.1, τ f =5.8 ppm/oC).The reaction sintering that the present invention uses eliminates pre-burning, secondary ball milling, granulation compared to traditional solid reaction process It with the series of steps such as dumping, further decreases production cost, simplify preparation process, be its commercially extensive and persistence Applications expanding road.
Summary of the invention
NaCa is prepared using reaction sintering the object of the present invention is to provide a kind of2Mg2V3O12The side of microwave dielectric ceramic Method.
Specific steps are as follows:
(1) with the Na of purity >=99%2CO3、CaCO3, MgO and V2O5High-purity powder is that raw material presses NaCa2Mg2V3O12Chemistry meter Amount obtains mixed powder, the ratio for being then 1:2:1 according to mixed powder, zirconia ball and dehydrated alcohol mass ratio than carrying out weighing Example sequentially adds zirconia ball and dehydrated alcohol into mixed powder, ball milling 4 hours, then dries at 100 ~ 120 DEG C, dries Powder afterwards is handled with the sieve sieving of 200 mesh.
(2) by powder obtained in step (1) be directly compressed into the case where no pre-burning diameter be 12mm, with a thickness of The cylindric sample of 6mm；Then sample is warming up to 775 ~ 875 DEG C with the heating rate of 5 DEG C/min, and the temperature is kept to be sintered 4 hours, obtain NaCa2Mg2V3O12Microwave dielectric ceramic.
The reaction sintering that the present invention uses is saving pre-burning, secondary ball milling, granulation compared to traditional solid reaction process There is fine and close microstructure, higher with successfully preparing two kinds in the case where the series of steps such as dumpingQ×fValue and nearly zero τ f The microwave-medium ceramics of value.It ensure that the performance of material while further reducing the cost, simplifying experimental implementation, have certain Application potential.
Specific embodiment
Embodiment 1:
(1) Na for being 99% with purity2CO3、CaCO3, MgO and V2O5High-purity powder is that raw material presses NaCa2Mg2V3O12Chemistry meter Amount obtains mixed powder, the ratio for being then 1:2:1 according to mixed powder, zirconia ball and dehydrated alcohol mass ratio than carrying out weighing Example sequentially adds zirconia ball and dehydrated alcohol into mixed powder, ball milling 4 hours, then dries at 110 DEG C, after drying Powder is handled with the sieve sieving of 200 mesh.
(2) by powder obtained in step (1) be directly compressed into the case where no pre-burning diameter be 12mm, with a thickness of The cylindric sample of 6mm；Then sample is warming up to 775 DEG C with the heating rate of 5 DEG C/min, and keeps temperature sintering 4 small When, obtain NaCa2Mg2V3O12Microwave dielectric ceramic.
Embodiment 2 ~ 5:
In addition to by the sintering temperature in step (2) according to being adjusted in table 1 other than, the preparation step of embodiment 2 ~ 5 is the same as implementing Example 1, specific sintering temperature are shown in Table 1.With cylindrical dielectric resonator method to LiCa made from embodiment 1 ~ 53ZnV3O12Micro-wave dielectric Ceramics carry out the evaluation of microwave dielectric property, and concrete outcome is shown in Table 1.
From experimental data it can be seen that this ceramics can be widely applied for the microwaves such as various medium substrates, antenna and filter electricity The manufacture of sub- component meets the technology needs of Modern Mobile Communications Systems.
The design parameter of 1 embodiment 1 ~ 5 of table

Claims (1)

1. a kind of NaCa2Mg2V3O12The preparation method of microwave dielectric ceramic, it is characterised in that specific steps are as follows:
(1) with the Na of purity >=99%2CO3、CaCO3, MgO and V2O5High-purity powder is that raw material presses NaCa2Mg2V3O12Stoichiometry Than carrying out weighing, mixed powder is obtained, the ratio for being then 1:2:1 according to mixed powder, zirconia ball and dehydrated alcohol mass ratio Zirconia ball and dehydrated alcohol are sequentially added into mixed powder, ball milling 4 hours, are then dried at 100 ~ 120 DEG C, after drying Powder handled with the sieve sievings of 200 mesh；
(2) powder obtained in step (1) is directly compressed into diameter in the case where no pre-burning is 12mm, with a thickness of 6mm Cylindric sample；Then sample is warming up to 775 ~ 875 DEG C with the heating rate of 5 DEG C/min, and keeps temperature sintering 4 small When, obtain NaCa2Mg2V3O12Microwave dielectric ceramic.
CN201811111699.3A 2018-09-24 2018-09-24 NaCa2Mg2V3O12The preparation method of microwave dielectric ceramic Pending CN109111226A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110357628A (en) * 2019-08-01 2019-10-22 电子科技大学 A kind of Ca5Mg4-xCox(VO4)6Low temperature sintering microwave ceramic material and preparation method thereof
CN112830515A (en) * 2021-01-19 2021-05-25 大连理工大学 NaMg with octahedral structure4V3O12Method for producing a material
CN113024249A (en) * 2021-03-29 2021-06-25 三峡大学 Microwave dielectric ceramic composite material and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5133129A (en) * 1988-12-27 1992-07-28 At&T Bell Laboratories Methods of producing microwave device
CN102153343A (en) * 2011-01-10 2011-08-17 天津大学 Method for preparing high Q-value magnesium titanate base microwave medium ceramics by adopting reactive sintering method
CN102861569A (en) * 2012-10-17 2013-01-09 桂林理工大学 Visible light responsive vanadium-containing garnet structural oxide photocatalyst and preparation method thereof
CN102887708A (en) * 2012-10-17 2013-01-23 桂林理工大学 Microwave dielectric ceramic NaCa2(Mg1-xZnx)2V3O12 capable of sintering at low temperature and preparation method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5133129A (en) * 1988-12-27 1992-07-28 At&T Bell Laboratories Methods of producing microwave device
CN102153343A (en) * 2011-01-10 2011-08-17 天津大学 Method for preparing high Q-value magnesium titanate base microwave medium ceramics by adopting reactive sintering method
CN102861569A (en) * 2012-10-17 2013-01-09 桂林理工大学 Visible light responsive vanadium-containing garnet structural oxide photocatalyst and preparation method thereof
CN102887708A (en) * 2012-10-17 2013-01-23 桂林理工大学 Microwave dielectric ceramic NaCa2(Mg1-xZnx)2V3O12 capable of sintering at low temperature and preparation method

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
LIANG FANG ET AL.: "A novel low firing microwave dielectric ceramic NaCa2Mg2V3O12", 《CERAMICS INTERNATIONAL》 *
YI-CHENG LIOU ET AL.: "Synthesis of BaTi4O9 ceramics by reaction-sintering process", 《MATERIALS RESEARCH BULLETIN》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110357628A (en) * 2019-08-01 2019-10-22 电子科技大学 A kind of Ca5Mg4-xCox(VO4)6Low temperature sintering microwave ceramic material and preparation method thereof
CN112830515A (en) * 2021-01-19 2021-05-25 大连理工大学 NaMg with octahedral structure4V3O12Method for producing a material
CN112830515B (en) * 2021-01-19 2022-04-12 大连理工大学 NaMg with octahedral structure4V3O12Method for producing a material
CN113024249A (en) * 2021-03-29 2021-06-25 三峡大学 Microwave dielectric ceramic composite material and preparation method thereof
CN113024249B (en) * 2021-03-29 2022-04-22 三峡大学 Microwave dielectric ceramic composite material and preparation method thereof

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