CN109251028A - A kind of low high Q lithium magnesium niobium series microwave dielectric ceramic and preparation method thereof that is situated between - Google Patents

A kind of low high Q lithium magnesium niobium series microwave dielectric ceramic and preparation method thereof that is situated between Download PDF

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CN109251028A
CN109251028A CN201811257438.2A CN201811257438A CN109251028A CN 109251028 A CN109251028 A CN 109251028A CN 201811257438 A CN201811257438 A CN 201811257438A CN 109251028 A CN109251028 A CN 109251028A
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张平
孙可欣
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Tianjin University
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Abstract

The invention belongs to technical field of ceramic material, disclose a kind of low high Q lithium magnesium niobium series microwave dielectric ceramic and preparation method thereof that is situated between, chemical formula Li3Mg2(Nb1‑xMox)O6+x/2, 0.02≤x≤0.08；It is by Li2CO3、MgO、Nb2O5、MoO3Ingredient in proportion；It dries, be sieved after ball milling, calcining obtains preburning powder at a certain temperature；It dries, be sieved after preburning powder secondary ball milling, be granulated, green body is pressed into after sieving；Green body is sintered at a certain temperature, and room temperature is down to after heat preservation and is obtained.The present invention uses conventional solid-state method, with Mo6+To Nb5+It is replaced, and introduces Lacking oxygen and keep charge balance, greatly improve Q*f value.Microwave-medium ceramics of the invention are nontoxic, pollution-free, meet environmental requirement；And preparation process is simple, and it is at low cost, it is suitable for large-scale production, to manufacture resonator, the microwave devices such as filter.

Description

A kind of low high Q lithium magnesium niobium series microwave dielectric ceramic and preparation method thereof that is situated between
Technical field
The invention belongs to technical field of ceramic material, and in particular to a kind of lithium magnesium niobium series microwave dielectric ceramic and its preparation side Method.
Background technique
With the rapid development of wireless communication technique, microwave-medium ceramics are because of its specific function in circuit and excellent spy Property causes more and more concerns.Microwave dielectric ceramic materials have low-k, low-loss, high resonant frequency stability The advantages that, the microwave devices such as resonator, filter, diectric antenna, dielectric guided wave circuit are mainly used as in microwave circuit.It grinds Study carefully Novel microwave dielectric ceramic and provides important materials for support for microwave circuit.
In recent years, the demand of electronic component high frequency development is growing, low dielectric microwave media ceramic becomes research Emphasis.Li3Mg2NbO6Microwave-medium ceramics are as a kind of novel low permittivity ceramic (εr< 20) it has received widespread attention, but should Ceramic systems Q*f value is lower, and Q*f value is 79,643GHz, higher energy loss is generated in microwave system application, so that micro- There is delay between the electric field and electric displacement vector of wave system system.
Therefore, in order to meet the needs of practical application, a kind of lithium magnesium niobium series microwave dielectric pottery of novel high Q*f value is studied Porcelain and preparation method thereof is particularly important.
Summary of the invention
The present invention is to solve existing Li3Mg2NbO6The lower technical problem of microwave-medium ceramics Q*f value, proposes one kind Low high Q lithium magnesium niobium series microwave dielectric ceramic and preparation method thereof that is situated between, using conventional solid-state method, with Mo6+To Nb5+It is replaced, and It introduces Lacking oxygen and keeps charge balance, greatly improve the Q*f value of lithium magnesium niobium series microwave dielectric ceramic.
In order to solve the above technical problems, the present invention is achieved by technical solution below:
A kind of low high Q lithium magnesium niobium series microwave dielectric ceramic that is situated between, chemical formula Li3Mg2(Nb1-xMox)O6+x/2, 0.02≤x ≤0.08。
Further, by Li2CO3、MgO、Nb2O5、MoO3Raw material is made.
A kind of preparation method of the low high Q lithium magnesium niobium series microwave dielectric ceramic that is situated between, this method follow the steps below:
(1) by Li2CO3、MgO、Nb2O5、MoO3Raw material, according to chemical formula Li3Mg2(Nb1-xMox)O6+x/2, 0.02≤x≤ 0.08 carries out ingredient；By gained ingredient, deionized water, abrading-ball according to the mass ratio of 2:16:15 the primary ball milling 4-8 on ball mill Hour；
(2) mix obtained by step (1) dried, cross 40 meshes, obtain evengranular mixed-powder；
(3) by mixed-powder obtained by step (2) 925-1000 DEG C temperature lower calcination 4-6 hours, be down to room temperature with furnace temperature After obtain preburning powder；
(4) by preburning powder, deionized water obtained by step (3), abrading-ball according to the mass ratio of 2:16:15 two on ball mill Secondary ball milling 6-8 hours；
(5) after the drying of powder obtained by step (4), 40 meshes being crossed, the paraffin conduct for accounting for its mass ratio 6-10wt% is added Adhesive is granulated, and is crossed 80 meshes and is pressed into green body later；
(6) green body obtained by step (5) is sintered at a temperature of 1150-1250 DEG C, keeps the temperature 4-6 hours, is down to room with furnace temperature A kind of low high Q lithium magnesium niobium series microwave dielectric ceramic that is situated between is obtained after temperature.
Preferably, the Ball-milling Time in step (1) is 8 hours.
Preferably, the calcination temperature in step (3) is 950 DEG C, and calcination time is 4 hours.
Preferably, the Ball-milling Time in step (4) is 8 hours.
Preferably, the mass ratio of paraffin is 8wt% in step (5).
Preferably, the sintering temperature in step (6) is 1200 DEG C.
The beneficial effects of the present invention are:
The present invention uses the Mo of different content6+Replace Nb5+, charge balance is kept by introducing Lacking oxygen, it is anti-using solid phase Method is answered to be prepared for a kind of low-loss, the novel lithium magnesium niobium series microwave dielectric ceramic Li suitable for 9-11GHz microwave frequency3Mg2 (Nb1-xMox)O6+x/2(0.02≤x≤0.08), with excellent microwave dielectric property, Q*f value can reach 84,845~ 116,266GHz, meanwhile, temperature coefficient of resonance frequency is with Mo6+The variation of doping increases to some extent.Work as x=0.02 When, prepared Li3Mg2(Nb0.98Mo0.02)O6.01Microwave-medium ceramics are sintered at 1200 DEG C, and heat preservation obtains optimal micro- for 6 hours Wave dielectric properties: εr~15.18, Q*f~116,266GHz, τf~-15.71ppm/ DEG C, Q*f value is greatly improved, is improved Temperature coefficient of resonance frequency.Microwave-medium ceramics of the invention are nontoxic, pollution-free, meet environmental requirement；And preparation process is simple, It is at low cost, it is suitable for large-scale production, to manufacture resonator, the microwave devices such as filter.
Specific embodiment
Below by specific embodiment, the present invention is described in further detail:
Following embodiment can make those skilled in the art that the present invention be more completely understood, but not limit this in any way Invention.
The chemical raw material Li that the present invention uses2CO3,MgO,Nb2O5,MoO3Purity is all larger than 99%, with Li3Mg2NbO6Ceramics For base-material, using the Mo of different content6+Replace Nb5+, and charge balance is kept by introducing Lacking oxygen, it prepares a kind of novel The low high Q lithium magnesium niobium series microwave dielectric ceramic that is situated between.
The present invention is by Li2CO3、MgO、Nb2O5、MoO3Raw material is according to chemical formula Li3Mg2(Nb1-xMox)O6+x/2(0.02≤x ≤ 0.08) ingredient is carried out；Gained ingredient, deionized water, abrading-ball are added in polyester tank according to the mass ratio of 2:16:15, in ball The grinding machine last time ball milling 4-8 hours；Gained mix, which is placed in baking oven, dries, crosses 40 meshes, obtains evengranular mixing Powder；Gained mixed-powder 925-1000 DEG C temperature lower calcination 4-6 hours, be cooled to room temperature to obtain preburning powder with furnace temperature； Gained preburning powder, deionized water, abrading-ball are according to the mass ratio of 2:16:15 secondary ball milling 6-8 hours on ball mill；Gained powder After end dries, crosses 40 meshes, the paraffin that addition accounts for its mass ratio 6-10wt% is granulated as adhesive, is crossed after 80 meshes Using powder compressing machine under the pressure of 4MPa by the powder pressing after granulation at diameter be 10mm, with a thickness of the green compact of 5mm；It will Green compact are sintered at a temperature of 1150-1250 DEG C, keep the temperature 4-6 hours, are cooled to room temperature to obtain a kind of novel low high Q lithium that is situated between with furnace temperature Magnesium niobium series microwave dielectric ceramic；Finally by Network Analyzer and the microwave dielectric property of dependence test fixture test article.
Embodiment 1:
1. according to microwave-medium ceramics component Li3Mg2(Nb0.98Mo0.02)O6.01, claim Li2CO3-6.8297g、MgO- 4.9671g、Nb2O5-8.0258g、MoO3- 0.1774g ingredient, total 20g；Mixed powder is added in polyester tank, and 160ml is added and goes After ionized water and 150g zirconium ball, primary ball milling 4 hours on planetary ball mill, drum's speed of rotation is 250 revs/min；
2. the raw material after ball milling is placed in drying box and dries and cross 40 meshes, evengranular powder is obtained；
3. powder is calcined 4 hours in 925 DEG C；
4. calcined powder, deionized water and zirconium ball are put into polyester tank according to the mass ratio of 2:16:15, secondary ball Mill 6 hours, is dried after discharging, crosses 40 meshes；Add and accounts for powder quality than being granulated for the paraffin of 6wt% as adhesive, so 80 meshes are crossed afterwards；Powder is pressed into for 10mm, with a thickness of the green body of 5mm by diameter with the pressure of 4MPa with powder compressing machine again；
5. green body is sintered in 1150 DEG C, 4 hours are kept the temperature, a kind of novel low high Q lithium magnesium niobium series microwave dielectric pottery that is situated between is made Porcelain；
Finally, the sample microwave property as obtained by Network Analyzer and the test of dependence test fixture.
Embodiment 2:
1. according to microwave-medium ceramics component Li3Mg2(Nb0.98Mo0.02)O6.01, claim Li2CO3-6.8297g、MgO- 4.9671g、Nb2O5-8.0258g、MoO3- 0.1774g ingredient, total 20g；Mixed powder is added in polyester tank, and 160ml is added and goes After ionized water and 150g zirconium ball, primary ball milling 6 hours on planetary ball mill, drum's speed of rotation is 250 revs/min；
2. the raw material after ball milling is placed in drying box and dries and cross 40 meshes, evengranular powder is obtained；
3. powder is calcined 6 hours in 925 DEG C；
4. calcined powder, deionized water and zirconium ball are put into polyester tank according to the mass ratio of 2:16:15, secondary ball Mill 8 hours, is dried after discharging, crosses 40 meshes；Add and accounts for powder quality than being granulated for the paraffin of 10wt% as adhesive, so 80 meshes are crossed afterwards；Powder is pressed into for 10mm, with a thickness of the green body of 5mm by diameter with the pressure of 4MPa with powder compressing machine again；
5. green body is sintered in 1150 DEG C, 6 hours are kept the temperature, a kind of novel low high Q lithium magnesium niobium series microwave dielectric pottery that is situated between is made Porcelain；
Finally, the sample microwave property as obtained by Network Analyzer and the test of dependence test fixture.
Embodiment 3:
1. according to microwave-medium ceramics component Li3Mg2(Nb0.98Mo0.02)O6.01, claim Li2CO3-6.8297g、MgO- 4.9671g、Nb2O5-8.0258g、MoO3- 0.1774g ingredient, total 20g；Mixed powder is added in polyester tank, and 160ml is added and goes After ionized water and 150g zirconium ball, primary ball milling 8 hours on planetary ball mill, drum's speed of rotation is 250 revs/min；
2. the raw material after ball milling is placed in drying box and dries and cross 40 meshes, evengranular powder is obtained；
3. powder is calcined 4 hours in 950 DEG C；
4. calcined powder, deionized water and zirconium ball are put into polyester tank according to the mass ratio of 2:16:15, secondary ball Mill 8 hours, is dried after discharging, crosses 40 meshes；Add and accounts for powder quality than being granulated for the paraffin of 8wt% as adhesive, so 80 meshes are crossed afterwards；Powder is pressed into for 10mm, with a thickness of the green body of 5mm by diameter with the pressure of 4MPa with powder compressing machine again；
5. green body is sintered in 1200 DEG C, 6 hours are kept the temperature, a kind of novel low high Q lithium magnesium niobium series microwave dielectric pottery that is situated between is made Porcelain；
Finally, the sample microwave property as obtained by Network Analyzer and the test of dependence test fixture.
Embodiment 4:
1. according to microwave-medium ceramics component Li3Mg2(Nb0.98Mo0.02)O6.01, claim Li2CO3-6.8297g、MgO- 4.9671g、Nb2O5-8.0258g、MoO3- 0.1774g ingredient, total 20g；Mixed powder is added in polyester tank, and 160ml is added and goes After ionized water and 150g zirconium ball, primary ball milling 8 hours on planetary ball mill, drum's speed of rotation is 250 revs/min；
2. the raw material after ball milling is placed in drying box and dries and cross 40 meshes, evengranular powder is obtained；
3. powder is calcined 5 hours in 1000 DEG C；
4. calcined powder, deionized water and zirconium ball are put into polyester tank according to the mass ratio of 2:16:15, secondary ball Mill 8 hours, is dried after discharging, crosses 40 meshes；Add and accounts for powder quality than being granulated for the paraffin of 8wt% as adhesive, so 80 meshes are crossed afterwards；Powder is pressed into for 10mm, with a thickness of the green body of 5mm by diameter with the pressure of 4MPa with powder compressing machine again；
5. green body is sintered in 1200 DEG C, 6 hours are kept the temperature, a kind of novel low high Q lithium magnesium niobium series microwave dielectric pottery that is situated between is made Porcelain；
Finally, the sample microwave property as obtained by Network Analyzer and the test of dependence test fixture.
Embodiment 5:
1. according to microwave-medium ceramics component Li3Mg2(Nb0.96Mo0.04)O6.02, claim Li2CO3-6.8251g、MgO- 4.9639g、Nb2O5-7.8569g、MoO3- 0.3545g ingredient, total 20g；Mixed powder is added in polyester tank, and 160ml is added and goes After ionized water and 150g zirconium ball, primary ball milling 6 hours on planetary ball mill, drum's speed of rotation is 250 revs/min；
2. the raw material after ball milling is placed in drying box and dries and cross 40 meshes, evengranular powder is obtained；
3. powder is calcined 4 hours in 950 DEG C；
4. calcined powder, deionized water and zirconium ball are put into polyester tank according to the mass ratio of 2:16:15, secondary ball Mill 6 hours, is dried after discharging, crosses 40 meshes；Add and accounts for powder quality than being granulated for the paraffin of 8wt% as adhesive, so 80 meshes are crossed afterwards；Powder is pressed into for 10mm, with a thickness of the green body of 5mm by diameter with the pressure of 4MPa with powder compressing machine again；
5. green body is sintered in 1225 DEG C, 6 hours are kept the temperature, a kind of novel low high Q lithium magnesium niobium series microwave dielectric pottery that is situated between is made Porcelain；
Finally, the sample microwave property as obtained by Network Analyzer and the test of dependence test fixture.
Embodiment 6:
1. according to microwave-medium ceramics component Li3Mg2(Nb0.96Mo0.04)O6.02, claim Li2CO3-6.8251g、MgO- 4.9639g、Nb2O5-7.8569g、MoO3- 0.3545g ingredient, total 20g；Mixed powder is added in polyester tank, and 160ml is added and goes After ionized water and 150g zirconium ball, primary ball milling 8 hours on planetary ball mill, drum's speed of rotation is 250 revs/min；
2. the raw material after ball milling is placed in drying box and dries and cross 40 meshes, evengranular powder is obtained；
3. powder is calcined 4 hours in 975 DEG C；
4. calcined powder, deionized water and zirconium ball are put into polyester tank according to the mass ratio of 2:16:15, secondary ball Mill 7 hours, is dried after discharging, crosses 40 meshes；Add and accounts for powder quality than being granulated for the paraffin of 6wt% as adhesive, so 80 meshes are crossed afterwards；Powder is pressed into for 10mm, with a thickness of the green body of 5mm by diameter with the pressure of 4MPa with powder compressing machine again；
5. green body is sintered in 1175 DEG C, 4 hours are kept the temperature, a kind of novel low high Q lithium magnesium niobium series microwave dielectric pottery that is situated between is made Porcelain；
Finally, the sample microwave property as obtained by Network Analyzer and the test of dependence test fixture.
Embodiment 7:
1. according to microwave-medium ceramics component Li3Mg2(Nb0.96Mo0.04)O6.02, claim Li2CO3-6.8251g、MgO- 4.9639g、Nb2O5-7.8569g、MoO3- 0.3545g ingredient, total 20g；Mixed powder is added in polyester tank, and 160ml is added and goes After ionized water and 150g zirconium ball, primary ball milling 6 hours on planetary ball mill, drum's speed of rotation is 250 revs/min；
2. the raw material after ball milling is placed in drying box and dries and cross 40 meshes, evengranular powder is obtained；
3. powder is calcined 4 hours in 975 DEG C；
4. calcined powder, deionized water and zirconium ball are put into polyester tank according to the mass ratio of 2:16:15, secondary ball Mill 6 hours, is dried after discharging, crosses 40 meshes；Add and accounts for powder quality than being granulated for the paraffin of 6wt% as adhesive, so 80 meshes are crossed afterwards；Powder is pressed into for 10mm, with a thickness of the green body of 5mm by diameter with the pressure of 4MPa with powder compressing machine again；
5. green body is sintered in 1200 DEG C, 6 hours are kept the temperature, a kind of novel low high Q lithium magnesium niobium series microwave dielectric pottery that is situated between is made Porcelain；
Finally, the sample microwave property as obtained by Network Analyzer and the test of dependence test fixture.
Embodiment 8:
1. according to microwave-medium ceramics component Li3Mg2(Nb0.94Mo0.06)O6.03, claim Li2CO3-6.8205g、MgO- 4.9607g、Nb2O5-7.6882g、MoO3- 0.5315g ingredient, total 20g；Mixed powder is added in polyester tank, and 160ml is added and goes After ionized water and 150g zirconium ball, primary ball milling 8 hours on planetary ball mill, drum's speed of rotation is 250 revs/min；
2. the raw material after ball milling is placed in drying box and dries and cross 40 meshes, evengranular powder is obtained；
3. powder is calcined 4 hours in 975 DEG C；
4. calcined powder, deionized water and zirconium ball are put into polyester tank according to the mass ratio of 2:16:15, secondary ball Mill 8 hours, is dried after discharging, crosses 40 meshes；Add and accounts for powder quality than being granulated for the paraffin of 8wt% as adhesive, so 80 meshes are crossed afterwards；Powder is pressed into for 10mm, with a thickness of the green body of 5mm by diameter with the pressure of 4MPa with powder compressing machine again；
5. green body is sintered in 1200 DEG C, 6 hours are kept the temperature, a kind of novel low high Q lithium magnesium niobium series microwave dielectric pottery that is situated between is made Porcelain；
Finally, the sample microwave property as obtained by Network Analyzer and the test of dependence test fixture.
Embodiment 9:
1. according to microwave-medium ceramics component Li3Mg2(Nb0.94Mo0.06)O6.03, claim Li2CO3-6.8205g、MgO- 4.9607g、Nb2O5-7.6882g、MoO3- 0.5315g ingredient, total 20g；Mixed powder is added in polyester tank, and 160ml is added and goes After ionized water and 150g zirconium ball, primary ball milling 6 hours on planetary ball mill, drum's speed of rotation is 250 revs/min；
2. the raw material after ball milling is placed in drying box and dries and cross 40 meshes, evengranular powder is obtained；
3. powder is calcined 4 hours in 1000 DEG C；
4. calcined powder, deionized water and zirconium ball are put into polyester tank according to the mass ratio of 2:16:15, secondary ball Mill 8 hours, is dried after discharging, crosses 40 meshes；Add and accounts for powder quality than being granulated for the paraffin of 8wt% as adhesive, so 80 meshes are crossed afterwards；Powder is pressed into for 10mm, with a thickness of the green body of 5mm by diameter with the pressure of 4MPa with powder compressing machine again；
5. green body is sintered in 1200 DEG C, 5 hours are kept the temperature, a kind of novel low high Q lithium magnesium niobium series microwave dielectric pottery that is situated between is made Porcelain；
Finally, the sample microwave property as obtained by Network Analyzer and the test of dependence test fixture.
Embodiment 10:
1. according to microwave-medium ceramics component Li3Mg2(Nb0.94Mo0.06)O6.03, claim Li2CO3-6.8205g、MgO- 4.9607g、Nb2O5-7.6882g、MoO3- 0.5315g ingredient, total 20g；Mixed powder is added in polyester tank, and 160ml is added and goes After ionized water and 150g zirconium ball, primary ball milling 8 hours on planetary ball mill, drum's speed of rotation is 250 revs/min；
2. the raw material after ball milling is placed in drying box and dries and cross 40 meshes, evengranular powder is obtained；
3. powder is calcined 4 hours in 1000 DEG C；
4. calcined powder, deionized water and zirconium ball are put into polyester tank according to the mass ratio of 2:16:15, secondary ball Mill 6 hours, is dried after discharging, crosses 40 meshes；Add and accounts for powder quality than being granulated for the paraffin of 10wt% as adhesive, so 80 meshes are crossed afterwards；Powder is pressed into for 10mm, with a thickness of the green body of 5mm by diameter with the pressure of 4MPa with powder compressing machine again；
5. green body is sintered in 1225 DEG C, 6 hours are kept the temperature, a kind of novel low high Q lithium magnesium niobium series microwave dielectric pottery that is situated between is made Porcelain；
Finally, the sample microwave property as obtained by Network Analyzer and the test of dependence test fixture.
Embodiment 11:
1. according to microwave-medium ceramics component Li3Mg2(Nb0.92Mo0.08)O6.04, claim Li2CO3-6.8158g、MgO- 4.9566g、Nb2O5-7.5185g、MoO3- 0.7801g ingredient, total 20g；Mixed powder is added in polyester tank, and 160ml is added and goes After ionized water and 150g zirconium ball, primary ball milling 4 hours on planetary ball mill, drum's speed of rotation is 250 revs/min；
2. the raw material after ball milling is placed in drying box and dries and cross 40 meshes, evengranular powder is obtained；
3. powder is calcined 4 hours in 1000 DEG C；
4. calcined powder, deionized water and zirconium ball are put into polyester tank according to the mass ratio of 2:16:15, secondary ball Mill 6 hours, is dried after discharging, crosses 40 meshes；Add and accounts for powder quality than being granulated for the paraffin of 10wt% as adhesive, so 80 meshes are crossed afterwards；Powder is pressed into for 10mm, with a thickness of the green body of 5mm by diameter with the pressure of 4MPa with powder compressing machine again；
5. green body is sintered in 1250 DEG C, 6 hours are kept the temperature, a kind of novel low high Q lithium magnesium niobium series microwave dielectric pottery that is situated between is made Porcelain；
Finally, the sample microwave property as obtained by Network Analyzer and the test of dependence test fixture.
Embodiment 12:
1. according to microwave-medium ceramics component Li3Mg2(Nb0.92Mo0.08)O6.04, claim Li2CO3-6.8158g、MgO- 4.9566g、Nb2O5-7.5185g、MoO3- 0.7801g ingredient, total 20g；Mixed powder is added in polyester tank, and 160ml is added and goes After ionized water and 150g zirconium ball, primary ball milling 6 hours on planetary ball mill, drum's speed of rotation is 250 revs/min；
2. the raw material after ball milling is placed in drying box and dries and cross 40 meshes, evengranular powder is obtained；
3. powder is calcined 4 hours in 975 DEG C；
4. calcined powder, deionized water and zirconium ball are put into polyester tank according to the mass ratio of 2:16:15, secondary ball Mill 8 hours, is dried after discharging, crosses 40 meshes；Add and accounts for powder quality than being granulated for the paraffin of 6wt% as adhesive, so 80 meshes are crossed afterwards；Powder is pressed into for 10mm, with a thickness of the green body of 5mm by diameter with the pressure of 4MPa with powder compressing machine again；
5. green body is sintered in 1225 DEG C, 5 hours are kept the temperature, a kind of novel low high Q lithium magnesium niobium series microwave dielectric pottery that is situated between is made Porcelain；
Finally, the sample microwave property as obtained by Network Analyzer and the test of dependence test fixture.
Embodiment 13:
1. according to microwave-medium ceramics component Li3Mg2(Nb0.92Mo0.08)O6.04, claim Li2CO3-6.8158g、MgO- 4.9566g、Nb2O5-7.5185g、MoO3- 0.7801g ingredient, total 20g；Mixed powder is added in polyester tank, and 160ml is added and goes After ionized water and 150g zirconium ball, primary ball milling 8 hours on planetary ball mill, drum's speed of rotation is 250 revs/min；
2. the raw material after ball milling is placed in drying box and dries and cross 40 meshes, evengranular powder is obtained；
3. powder is calcined 4 hours in 1000 DEG C；
4. calcined powder, deionized water and zirconium ball are put into polyester tank according to the mass ratio of 2:16:15, secondary ball Mill 8 hours, is dried after discharging, crosses 40 meshes；Add and accounts for powder quality than being granulated for the paraffin of 8wt% as adhesive, so 80 meshes are crossed afterwards；Powder is pressed into for 10mm, with a thickness of the green body of 5mm by diameter with the pressure of 4MPa with powder compressing machine again；
5. green body is sintered in 1250 DEG C, 6 hours are kept the temperature, a kind of novel low high Q lithium magnesium niobium series microwave dielectric pottery that is situated between is made Porcelain；
Finally, the sample microwave property as obtained by Network Analyzer and the test of dependence test fixture.
Embodiment 14 (comparative example):
1. according to microwave-medium ceramics component Li3Mg2NbO6, claim Li2CO3-6.8344g、MgO-4.9705g、Nb2O5- 8.1951g ingredient, total 20g；Mixed powder is added in polyester tank, after 160ml deionized water and 150g zirconium ball is added, planetary Ball mill last time ball milling 8 hours, drum's speed of rotation are 250 revs/min；
2. the raw material after ball milling is placed in drying box and dries and cross 40 meshes, evengranular powder is obtained；
3. powder is calcined 4 hours in 950 DEG C；
4. calcined powder, deionized water and zirconium ball are put into polyester tank according to the mass ratio of 2:16:15, secondary ball Mill 8 hours, is dried after discharging, crosses 40 meshes；Then the paraffin of additional 8wt% is granulated as adhesive, then crosses 80 mesh Sieve；Diameter is pressed into for 10mm, with a thickness of the green body of 5mm with the pressure of 4MPa with powder compressing machine again；
5. green body is sintered in 1150 DEG C, 6 hours are kept the temperature, a kind of novel low high Q lithium magnesium niobium series microwave dielectric pottery that is situated between is made Porcelain；
Finally, the sample microwave property as obtained by Network Analyzer and the test of dependence test fixture.
The detection method of 1-14 of the embodiment of the present invention is as follows:
1. the diameter and thickness of sample uses miking.
2. measuring institute respectively using open type chamber parallel plate method and enclosed cell method by Agilent 8720ES Network Analyzer The dielectric constant and Q*f value for preparing cylindrical ceramic material, gained ceramics are placed in test fixture and are put into ESPEC MC-710F Type high/low temperature recycles the measurement that incubator carries out temperature coefficient of resonance frequency, and temperature range is 25-85 DEG C, and test frequency range is 7- 13GHz。
Table 1 is Li in the present invention3Mg2(Nb1-xMox)O6+x/2, each embodiment related process parameters of the ceramics of 0.02≤x≤0.08 And microwave dielectric property.
Table 1
Have well from can be seen that the novel lithium magnesium niobium series microwave dielectric ceramic studied in the present invention in above-described embodiment Microwave dielectric property, with pure phase Li3Mg2NbO6Microwave-medium ceramics (embodiment 14) are compared, and whole Q*f value significantly improves, Meanwhile temperature coefficient of resonance frequency is with Mo6+The variation of doping increases to some extent.In conclusion as x=0.02, It is sintered at 1200 DEG C, keeps the temperature 6 hours (embodiment 3), gained ceramic performance is the most excellent: εr=15.18, Q*f=116, 266GHz,τf=-15.71ppm/ DEG C, significantly improve the microwave dielectric property of lithium magnesium niobium series microwave dielectric ceramic.
Although the preferred embodiment of the present invention is described above, the invention is not limited to above-mentioned specific Embodiment, the above mentioned embodiment is only schematical, is not restrictive, those skilled in the art Under the inspiration of the present invention, it when not departing from invention objective and scope of the claimed protection, can also make very much The specific transformation of form, within these are all belonged to the scope of protection of the present invention.

Claims (8)

1. a kind of low high Q lithium magnesium niobium series microwave dielectric ceramic that is situated between, which is characterized in that its chemical formula is Li3Mg2(Nb1-xMox) O6+x/2, 0.02≤x≤0.08.
2. the low high Q lithium magnesium niobium series microwave dielectric ceramic that is situated between of one kind according to claim 1, which is characterized in that by Li2CO3、 MgO、Nb2O5、MoO3Raw material is made.
3. a kind of preparation method of the low high Q lithium magnesium niobium series microwave dielectric ceramic that is situated between, which is characterized in that this method is according to the following steps It carries out:
(1) by Li2CO3、MgO、Nb2O5、MoO3Raw material, according to chemical formula Li3Mg2(Nb1-xMox)O6+x/2, 0.02≤x≤0.08 into Row ingredient；By gained ingredient, deionized water, abrading-ball according to the mass ratio of 2:16:15 primary ball milling 4-8 hours on ball mill；
(2) mix obtained by step (1) dried, cross 40 meshes, obtain evengranular mixed-powder；
(3) by mixed-powder obtained by step (2) 925-1000 DEG C temperature lower calcination 4-6 hours, be cooled to room temperature with furnace temperature To preburning powder；
(4) by preburning powder, deionized water obtained by step (3), abrading-ball according to the mass ratio of 2:16:15 the secondary ball on ball mill Mill 6-8 hours；
(5) after the drying of powder obtained by step (4), 40 meshes being crossed, the paraffin for accounting for its mass ratio 6-10wt% is added as bonding Agent is granulated, and is crossed 80 meshes and is pressed into green body later；
(6) green body obtained by step (5) is sintered at a temperature of 1150-1250 DEG C, keeps the temperature 4-6 hours, is cooled to room temperature with furnace temperature Obtain a kind of low high Q lithium magnesium niobium series microwave dielectric ceramic that is situated between.
4. the preparation method of the low high Q lithium magnesium niobium series microwave dielectric ceramic that is situated between of one kind according to claim 3, feature exist In the Ball-milling Time in step (1) is 8 hours.
5. the preparation method of the low high Q lithium magnesium niobium series microwave dielectric ceramic that is situated between of one kind according to claim 3, feature exist In the calcination temperature in step (3) is 950 DEG C, and calcination time is 4 hours.
6. the preparation method of the low high Q lithium magnesium niobium series microwave dielectric ceramic that is situated between of one kind according to claim 3, feature exist In the Ball-milling Time in step (4) is 8 hours.
7. the preparation method of the low high Q lithium magnesium niobium series microwave dielectric ceramic that is situated between of one kind according to claim 3, feature exist In the mass ratio of paraffin is 8wt% in step (5).
8. the preparation method of the low high Q lithium magnesium niobium series microwave dielectric ceramic that is situated between of one kind according to claim 3, feature exist In the sintering temperature in step (6) is 1200 DEG C.
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