CN107382317A - A kind of magnesium nickel zirconium niobium series microwave dielectric ceramic - Google Patents

A kind of magnesium nickel zirconium niobium series microwave dielectric ceramic Download PDF

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CN107382317A
CN107382317A CN201710632156.5A CN201710632156A CN107382317A CN 107382317 A CN107382317 A CN 107382317A CN 201710632156 A CN201710632156 A CN 201710632156A CN 107382317 A CN107382317 A CN 107382317A
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microwave dielectric
dielectric ceramic
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magnesium nickel
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肖谧
娄捷
韦艳双
顾青青
周子淇
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Tianjin University
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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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    • 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
    • C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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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
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
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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
    • C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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Abstract

The invention discloses a kind of magnesium nickel zirconium niobium series microwave dielectric ceramic and preparation method thereof, consisting of Mg1‑xNixZrNb2O8(0<x≤0.12).First by MgO, NiO, ZrO2、Nb2O5By Mg1‑ xNixZrNb2O8(0<X≤0.12) dispensing is carried out, by abrading-ball, drying, sieving, in 1100 DEG C of pre-burnings；Additional 8% percentage by weight paraffin is granulated after secondary ball milling, drying again, re-compacted to be shaped to base substrate, and high-performance magnesium nickel zirconium niobium series microwave dielectric ceramic is made in 1260~1300 DEG C of sintering in base substrate.The present invention successfully obtains Q × f up to 74534.1GHz, dielectric constant 24.5768, and temperature coefficient of resonance frequency is 49.1124ppm/ DEG C of high performance microwave media ceramic.Preparation technology of the present invention is simple, and process is pollution-free, is a kind of microwave dielectric material of up-and-coming millimetre-wave circuit.

Description

A kind of magnesium nickel zirconium niobium series microwave dielectric ceramic
Technical field
The invention belongs to a kind of ceramic composition characterized by composition, and more particularly to one kind is with magnesium zirconium niobium series microwave dielectric Based on ceramics, substitute magnesium ion with nickel ion, prepare high quality factor magnesium nickel zirconium niobium series microwave dielectric ceramic and its preparation side Method.
Background technology
With the fast development of microwave communication cause, mobile communication, automobile telephone, telstar, military radar, the whole world are fixed The position field such as system and portable phone increasingly increases to the demand of miniaturization, the microwave circuit of high performance and microwave device Add, this requires to continually develop the new material with more superior function.Microwave-medium ceramics refer in microwave frequency band circuit Middle one kind ceramics that microwave signal process is completed as dielectric material, for manufacturing smaller device and improving microwave integrated circuit Packaging density it is highly effective.For making the media ceramic of the devices such as dielectric resonator, wave filter, following condition must be met： Higher dielectric constant (εr) to realize the miniaturization of device and improve integrated level, compared with low-dielectric loss (dielectric loss tangent angle Tan δ) to improve selecting frequency characteristic, level off to zero temperature coefficient of resonance frequency (τf) to improve temperature stability.
Ceramic compound MgZrNb with wolframite structure2O8Media ceramic has obtained relatively broad concern, with this Dielectric material based on kind ceramic compound can preferably meet high-k, low-dielectric loss and low resonant frequency temperature The requirement of coefficient.India V.R.K.Murthy reports MgZrNb2O8Its ceramic dielectric constant of system is 9.6, and quality factor are 58500GHz, temperature coefficient of resonance frequency are -31.5ppm/ DEG C.
The content of the invention
The purpose of the present invention, it is further to improve magnesium zirconium niobium (MgZrNb in prior art basis2O8) series microwave dielectric The microwave dielectric property of ceramics, with MgO, NiO, ZrO2、Nb2O5For primary raw material, preparing one kind has superior microwave dielectric property The novel magnesium nickel zirconium niobium series microwave dielectric ceramic of energy：Mg1-xNixZrNb2O8Microwave-medium ceramics, wherein 0<x≤0.12.
The present invention is achieved by following technical solution.
A kind of magnesium nickel zirconium niobium series microwave dielectric ceramic, consisting of Mg1-xNixZrNb2O8, wherein 0<x≤0.12.
The preparation method of above-mentioned magnesium nickel zirconium niobium system microwave ceramics, has steps of：
(1) by MgO, NiO, ZrO2、Nb2O5Raw material, by chemical formula Mg1-xNixZrNb2O8, wherein 0<Matched somebody with somebody x≤0.12 Material, powder is put into ball grinder, adds deionized water and zirconia ball, ball milling 6 hours on ball mill；
(2) raw material after step (1) ball milling is placed in 110 DEG C of drying, after raw material drying, crosses 40 mesh sieves, obtain particle Uniform powder；
(3) powder that step (2) is well mixed is fitted into crucible and is placed in high temperature furnace, in 1100 DEG C of pre-burnings 2 hours；
(4) ceramic powder after step (3) pre-burning is put into ball grinder, deionized water and zirconia ball is added, in ball Secondary ball milling 6 hours on grinding machine, and in 110 DEG C of drying；After the drying in ceramic powder additional 8% percentage by weight paraffin It is granulated, crosses 60 mesh sieves, then compressing with powder compressing machine is base substrate；
(5) base substrate of step (4) is incubated 4 hours, magnesium nickel zirconium niobium series microwave dielectric is made in 1260-1300 DEG C of sintering Ceramics.
The x=0.08 of the step (1).
MgO, NiO, ZrO of the step (1)2、Nb2O5The quality purity of raw material is more than 99.9%.
The step (1), the raw material of step (4) ball-milling technology, the mass ratio of deionized water and abrading-ball are 2:16:15.
The step (1), the ball mill of step (4) are planetary ball mill.
The pressure of the powder compressing machine of the step (4) is 6Mpa.
The blank diameter of the step (4) is 10mm, thickness 5mm.
The sintering temperature of the step (5) is 1280 DEG C, soaking time 4 hours.
The present invention is with MgZrNb2O8Based on microwave-medium ceramics, taking for certain content is carried out with Ni ion pair Mg ions In generation, successfully obtain the higher microwave-medium ceramics Mg of microwave dielectric property1-xNixZrNb2O8(x=0.08), its quality because Number reaches 74534.1GHz, dielectric constant 24.5768, and temperature coefficient of resonance frequency is -49.1124ppm/ DEG C, and sintering temperature is 1280℃.The preparation technology of the present invention is simple, and process is pollution-free, and microwave dielectric property is excellent, is a kind of up-and-coming millimeter Wave circuit microwave dielectric material.
Embodiment
The present invention is more than 99.9% chemical raw material MgO, NiO, ZrO using purity2、Nb2O5, prepare Mg1-xNixZrNb2O8 (0<X≤0.12) microwave-medium ceramics.Specific embodiment is as follows.
Embodiment 1
1. according to microwave-medium ceramics component Mg1-xNixZrNb2O8(x=0.02) MgO-1.8372g, NiO-, are weighed 0.0695g、ZrO2-5.7307g、Nb2O5- 12.3626g dispensings, common 20g；Mixed powder is added in ball grinder, is added 160ml and is gone After ionized water and 150g zirconium balls, ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min；
Dried 2. the raw material after ball milling is placed under 110 DEG C of temperature conditionss, cross 40 mesh sieves, obtain evengranular powder；
3. evengranular powder is calcined 2 hours in 1100 DEG C；
4. the powder after calcining is put into ball grinder, deionized water and zirconia ball are added, secondary ball milling 6 hours, is gone out Dried after material under 110 DEG C of temperature conditionss, the paraffin for then adding 8% percentage by weight is granulated, and crosses 60 mesh sieves；Use again Powder compressing machine is pressed into a diameter of 10mm with 6Mpa pressure, and thickness is 5mm base substrate；
5. base substrate is incubated 4 hours, high-performance magnesium nickel zirconium niobium series microwave dielectric ceramic is made in 1280 DEG C of sintering；
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 Mg1-xNixZrNb2O8(x=0.04) MgO-1.7969g, NiO-, are weighed 0.1387g、ZrO2-5.7215g、Nb2O5- 12.3429g dispensings, common 20g；Mixed powder is added in ball grinder, is added 160ml and is gone After ionized water and 150g zirconium balls, ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min；
Dried 2. the raw material after ball milling is placed under 110 DEG C of temperature conditionss, cross 40 mesh sieves, obtain evengranular powder；
3. evengranular powder is calcined 2 hours in 1100 DEG C；
4. the powder after calcining is put into ball grinder, deionized water and zirconia ball are added, secondary ball milling 6 hours, is gone out Dried after material under 110 DEG C of temperature conditionss, the paraffin for then adding 8% percentage by weight is granulated, and crosses 60 mesh sieves；Use again Powder compressing machine is pressed into a diameter of 10mm with 6Mpa pressure, and thickness is 5mm base substrate；
5. base substrate is incubated 4 hours, high-performance magnesium nickel zirconium niobium series microwave dielectric ceramic is made in 1280 DEG C of sintering；
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 Mg1-xNixZrNb2O8(x=0.06) MgO-1.7566g, NiO-, are weighed 0.2078g、ZrO2-5.7124g、Nb2O5- 12.3232g dispensings, common 20g；Mixed powder is added in ball grinder, is added 160ml and is gone After ionized water and 150g zirconium balls, ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min；
Dried 2. the raw material after ball milling is placed under 110 DEG C of temperature conditionss, cross 40 mesh sieves, obtain evengranular powder；
3. evengranular powder is calcined 2 hours in 1100 DEG C；
4. the powder after calcining is put into ball grinder, deionized water and zirconia ball are added, secondary ball milling 6 hours, is gone out Dried after material under 110 DEG C of temperature conditionss, the paraffin for then adding 8% percentage by weight is granulated, and crosses 60 mesh sieves；Use again Powder compressing machine is pressed into a diameter of 10mm with 6Mpa pressure, and thickness is 5mm base substrate；
5. base substrate is incubated 4 hours, high-performance magnesium nickel zirconium niobium series microwave dielectric ceramic is made in 1280 DEG C of sintering；
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 Mg1-xNixZrNb2O8(x=0.08) MgO-1.7165g, NiO-, are weighed 0.2766g、ZrO2-5.7033g、Nb2O5- 12.3036g dispensings, common 20g；Mixed powder is added in ball grinder, is added 160ml and is gone After ionized water and 150g zirconium balls, ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min；
Dried 2. the raw material after ball milling is placed under 110 DEG C of temperature conditionss, cross 40 mesh sieves, obtain evengranular powder；
3. evengranular powder is calcined 2 hours in 1100 DEG C；
4. the powder after calcining is put into ball grinder, deionized water and zirconia ball are added, secondary ball milling 6 hours, is gone out Dried after material under 110 DEG C of temperature conditionss, the paraffin for then adding 8% percentage by weight is granulated, and crosses 60 mesh sieves；Use again Powder compressing machine is pressed into a diameter of 10mm with 6Mpa pressure, and thickness is 5mm base substrate；
5. base substrate is incubated 4 hours, high-performance magnesium nickel zirconium niobium series microwave dielectric ceramic is made in 1280 DEG C of sintering；
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 Mg1-xNixZrNb2O8(x=0.10) MgO-1.6765g, NiO-, are weighed 0.3452g、ZrO2-5.6942g、Nb2O5- 12.2841g dispensings, common 20g；Mixed powder is added in ball grinder, is added 160ml and is gone After ionized water and 150g zirconium balls, ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min；
Dried 2. the raw material after ball milling is placed under 110 DEG C of temperature conditionss, cross 40 mesh sieves, obtain evengranular powder；
3. evengranular powder is calcined 2 hours in 1100 DEG C；
4. the powder after calcining is put into ball grinder, deionized water and zirconia ball are added, secondary ball milling 6 hours, is gone out Dried after material under 110 DEG C of temperature conditionss, the paraffin for then adding 8% percentage by weight is granulated, and crosses 60 mesh sieves；Use again Powder compressing machine is pressed into a diameter of 10mm with 6Mpa pressure, and thickness is 5mm base substrate；
5. base substrate is incubated 4 hours, high-performance magnesium nickel zirconium niobium series microwave dielectric ceramic is made in 1280 DEG C of sintering；
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 Mg1-xNixZrNb2O8(x=0.12) MgO-1.6367g, NiO-, are weighed 0.4135g、ZrO2-5.6852g、Nb2O5- 12.2646g dispensings, common 20g；Mixed powder is added in ball grinder, is added 160ml and is gone After ionized water and 150g zirconium balls, ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min；
Dried 2. the raw material after ball milling is placed under 110 DEG C of temperature conditionss, cross 40 mesh sieves, obtain evengranular powder；
3. evengranular powder is calcined 2 hours in 1100 DEG C；
4. the powder after calcining is put into ball grinder, deionized water and zirconia ball are added, secondary ball milling 6 hours, is gone out Dried after material under 110 DEG C of temperature conditionss, the paraffin for then adding 8% percentage by weight is granulated, and crosses 60 mesh sieves；Use again Powder compressing machine is pressed into a diameter of 10mm with 6Mpa pressure, and thickness is 5mm base substrate；
5. base substrate is incubated 4 hours, high-performance magnesium nickel zirconium niobium series microwave dielectric ceramic is made in 1280 DEG C of sintering；
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 Mg1-xNixZrNb2O8(x=0.08) MgO-1.7165g, NiO-, are weighed 0.2766g、ZrO2-5.7033g、Nb2O5- 12.3036g dispensings, common 20g；Mixed powder is added in ball grinder, is added 160ml and is gone After ionized water and 150g zirconium balls, ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min；
Dried 2. the raw material after ball milling is placed under 110 DEG C of temperature conditionss, cross 40 mesh sieves, obtain evengranular powder；
3. evengranular powder is calcined 2 hours in 1100 DEG C；
4. the powder after calcining is put into ball grinder, deionized water and zirconia ball are added, secondary ball milling 6 hours, is gone out Dried after material under 110 DEG C of temperature conditionss, the paraffin for then adding 8% percentage by weight is granulated, and crosses 60 mesh sieves；Use again Powder compressing machine is pressed into a diameter of 10mm with 6Mpa pressure, and thickness is 5mm base substrate；
5. base substrate is incubated 4 hours, high-performance magnesium nickel zirconium niobium series microwave dielectric ceramic is made in 1260 DEG C of sintering；
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 Mg1-xNixZrNb2O8(x=0.08) MgO-1.7165g, NiO-, are weighed 0.2766g、ZrO2-5.7033g、Nb2O5- 12.3036g dispensings, common 20g；Mixed powder is added in ball grinder, is added 160ml and is gone After ionized water and 150g zirconium balls, ball milling 6 hours on planetary ball mill, drum's speed of rotation is 1000 revs/min；
Dried 2. the raw material after ball milling is placed under 110 DEG C of temperature conditionss, cross 40 mesh sieves, obtain evengranular powder；
3. evengranular powder is calcined 2 hours in 1100 DEG C；
4. the powder after calcining is put into ball grinder, deionized water and zirconia ball are added, secondary ball milling 6 hours, is gone out Dried after material under 110 DEG C of temperature conditionss, the paraffin for then adding 8% percentage by weight is granulated, and crosses 60 mesh sieves；Use again Powder compressing machine is pressed into a diameter of 10mm with 6Mpa pressure, and thickness is 5mm base substrate；
5. base substrate is incubated 4 hours, high-performance magnesium nickel zirconium niobium series microwave dielectric ceramic is made in 1300 DEG C of sintering；
Finally, the sample microwave property as obtained by Network Analyzer and the test of dependence test fixture.
The detection method of the specific embodiment of the invention is as follows:
1. by Agilent 8720ES Network Analyzers, using starting to rob cylindrical ceramic prepared by parallel plate method measurement The dielectric constant of material, test fixture is put into ESPEC MC-710F types high/low temperature circulation incubator and carries out resonant frequency temperature system Several measurements, temperature range are 25-85 DEG C of test frequency in the range of 6-15GHz.
2. using the quality factor of cylindrical ceramic sample prepared by the measurement of enclosed cell method.
The every key parameter and its dielectric properties testing result of the specific embodiment of the invention refer to table 1.
Table 1

Claims (8)

  1. A kind of 1. magnesium nickel zirconium niobium series microwave dielectric ceramic, consisting of Mg1-xNixZrNb2O8, wherein 0<x≤0.12.
    The preparation method of above-mentioned magnesium nickel zirconium niobium system microwave ceramics, has steps of：
    (1) by MgO, NiO, ZrO2、Nb2O5Raw material, by chemical formula Mg1-xNixZrNb2O8, wherein 0<X≤0.12 carries out dispensing, will Powder is put into ball grinder, adds deionized water and zirconia ball, ball milling 6 hours on ball mill；
    (2) raw material after step (1) ball milling is placed in 110 DEG C of drying, after raw material drying, crosses 40 mesh sieves, it is uniform to obtain particle Powder；
    (3) powder that step (2) is well mixed is fitted into crucible and is placed in high temperature furnace, in 1100 DEG C of pre-burnings 2 hours；
    (4) ceramic powder after step (3) pre-burning is put into ball grinder, deionized water and zirconia ball is added, in ball mill Upper secondary ball milling 6 hours, and in 110 DEG C of drying；The paraffin of additional 8% percentage by weight is carried out in ceramic powder after the drying It is granulated, crosses 60 mesh sieves, then compressing with powder compressing machine is base substrate；
    (5) base substrate of step (4) is incubated 4 hours, magnesium nickel zirconium niobium series microwave dielectric ceramic is made in 1260-1300 DEG C of sintering.
  2. A kind of 2. magnesium nickel zirconium niobium series microwave dielectric ceramic according to claim 1, it is characterised in that the x=of the step (1) 0.08。
  3. A kind of 3. magnesium nickel zirconium niobium series microwave dielectric ceramic according to claim 1, it is characterised in that the MgO of the step (1), NiO、ZrO2、Nb2O5The quality purity of raw material is more than 99.9%.
  4. 4. a kind of magnesium nickel zirconium niobium series microwave dielectric ceramic according to claim 1, it is characterised in that the step (1), step (4) mass ratio of the raw material of ball-milling technology, deionized water and abrading-ball is 2:16:15.
  5. 5. a kind of magnesium nickel zirconium niobium series microwave dielectric ceramic according to claim 1, it is characterised in that the step (1), step (4) ball mill is planetary ball mill.
  6. A kind of 6. magnesium nickel zirconium niobium series microwave dielectric ceramic according to claim 1, it is characterised in that the powder of the step (4) The pressure of tablet press machine is 6Mpa.
  7. A kind of 7. magnesium nickel zirconium niobium series microwave dielectric ceramic according to claim 1, it is characterised in that the base substrate of the step (4) A diameter of 10mm, thickness 5mm.
  8. A kind of 8. magnesium nickel zirconium niobium series microwave dielectric ceramic according to claim 1, it is characterised in that the sintering of the step (5) Temperature is 1280 DEG C, soaking time 4 hours.
CN201710632156.5A 2017-07-28 2017-07-28 A kind of magnesium nickel zirconium niobium series microwave dielectric ceramic Pending CN107382317A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107879739A (en) * 2017-12-07 2018-04-06 天津大学 A kind of magnesium cobalt zirconium niobium series microwave dielectric ceramic and preparation method thereof
CN109336596A (en) * 2018-09-30 2019-02-15 天津大学 Magnesium zirconium germanium niobium series microwave dielectric ceramic and preparation method and application with low-k and ultralow dielectric loss
CN109354495A (en) * 2018-09-30 2019-02-19 天津大学 Magnesium zirconium niobium antimony series microwave dielectric ceramic and preparation method and application
CN112851346A (en) * 2021-02-25 2021-05-28 电子科技大学 Ultra-low-loss zirconium magnesium niobate system microwave dielectric ceramic material and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107879739A (en) * 2017-12-07 2018-04-06 天津大学 A kind of magnesium cobalt zirconium niobium series microwave dielectric ceramic and preparation method thereof
CN109336596A (en) * 2018-09-30 2019-02-15 天津大学 Magnesium zirconium germanium niobium series microwave dielectric ceramic and preparation method and application with low-k and ultralow dielectric loss
CN109354495A (en) * 2018-09-30 2019-02-19 天津大学 Magnesium zirconium niobium antimony series microwave dielectric ceramic and preparation method and application
CN112851346A (en) * 2021-02-25 2021-05-28 电子科技大学 Ultra-low-loss zirconium magnesium niobate system microwave dielectric ceramic material and preparation method thereof

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Application publication date: 20171124