CN106518051A - Temperature-stable microwave dielectric ceramic material and preparation method thereof - Google Patents

Temperature-stable microwave dielectric ceramic material and preparation method thereof Download PDF

Info

Publication number
CN106518051A
CN106518051A CN201610969200.7A CN201610969200A CN106518051A CN 106518051 A CN106518051 A CN 106518051A CN 201610969200 A CN201610969200 A CN 201610969200A CN 106518051 A CN106518051 A CN 106518051A
Authority
CN
China
Prior art keywords
powder
hours
temperature
microwave
microwave dielectric
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201610969200.7A
Other languages
Chinese (zh)
Other versions
CN106518051B (en
Inventor
周焕福
谭祥虎
黄瑾
陈秀丽
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guilin University of Technology
Original Assignee
Guilin University of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Guilin University of Technology filed Critical Guilin University of Technology
Priority to CN201610969200.7A priority Critical patent/CN106518051B/en
Publication of CN106518051A publication Critical patent/CN106518051A/en
Application granted granted Critical
Publication of CN106518051B publication Critical patent/CN106518051B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • 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
    • C04B35/01—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
    • C04B35/46—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 titanium oxides or titanates
    • C04B35/462—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 titanium oxides or titanates based on titanates
    • C04B35/465—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 titanium oxides or titanates based on titanates based on alkaline earth metal titanates
    • C—CHEMISTRY; METALLURGY
    • 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
    • C—CHEMISTRY; METALLURGY
    • 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
    • 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
    • C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
    • C04B2235/3203—Lithium oxide or oxide-forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C—CHEMISTRY; METALLURGY
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Insulating Materials (AREA)

Abstract

The invention discloses a low-cost low-density temperature-stable microwave dielectric ceramic material and a preparation method thereof. The chemical composition formula of the microwave dielectric ceramic material is Li2O-3MgO-mTiO2 (4.1<=m<=6). The preparation method comprises the following steps: weighing high-purity powder Li2CO3, MgO and TiO2 according to a stoichiometric ratio of Li2O-3MgO-mTiO2 (4.1<=m<=6), wherein the purity of the high-purity powder is no less than 99%; performing wet ball milling and mixing on the raw materials in the step (1) for 4 hours, drying, and then respectively presintering at 900-950 DEG C for 4 hours; and finally, performing secondary ball milling on the presintered powder, adding 5wt% polyvinyl alcohol, granulating, then performing pressure molding, discharging batch from a green body, and sintering at 950-1300 DEG C for 4 hours. The microwave dielectric ceramic prepared by the invention has a moderate dielectric constant, a higher Q*f value and a near-zero tao f value, thereby having great commercial application prospects.

Description

A kind of temperature-stabilized microwave medium ceramic material and preparation method thereof
Technical field
The invention belongs to electronic ceramics and its manufacture field, the resonator that is related to use in microwave frequency band, wave filter, medium The preparation method of the dielectric ceramic materials of microwave device such as antenna, medium wave circuit.
Background technology
Microwave dielectric material refers to and is applied in microwave frequency band (300MHz～300GHz) circuit as medium and completes one The ceramics of kind or several functions, mainly for the preparation of the microwaves such as resonator, wave filter, diectric antenna, medium wave circuit unit device Part.In recent years, as microwave device constantly develops to cost degradation, miniaturization and lightweight direction, it is desirable to microwave-medium Material must have excellent microwave dielectric property (high Q × f values, moderate dielectric constant, nearly zero τfValue), low production into Originally, low density.Although commercial microwave dielectric ceramic materials are with excellent performance, such as Ba (Zn at present1/3Nb2/3)O3, Ba (Mg1/3Nb2/3)O3, Ba (Y1/2Ta1/2)O3, but high sintering temperature and density, expensive raw materials for production limit which in business On further apply.Therefore, the raw materials for production from low price prepare the microwave dielectric material of low cost, sintering temperature and low It has been trend of the times.But the difficulty of the material that searching meets above standard is very big, so some researcher exists Inexpensive, low-density material is found in the excellent material system of existing microwave dielectric property to carry out cooling process to reach mesh 's.The method of reduction sintering temperature the most frequently used at present mainly has following three kinds：(1) add sintering aid；(2) use superfine powder Body；(3) using the raw material of low melting point.But addition sintering aid will severe exacerbation material performance, using superfine powder will Increase production cost, so Many researchers concentrate on using the raw material of low melting point research direction to realize in low-temperature sintering.
Li2Mg3Ti4O12Ceramics have excellent microwave dielectric property (εr=20.2, Q × f=62300GHz, τf= 27.1ppm/℃)【Zhou H.F.,Liu X.B.,Chen X.L.,et al.Preparation,phase structure and microwave dielectric properties of a new low cost MgLi2/3Ti4/ 3O4compound.Materials Chemistry&Physics,2012,137(1):22-25】, low cost of material and compared with The features such as low density, but higher sintering temperature (1250 DEG C) limit its commercial extensive and persistence should With.TiO2With high dielectric constant and positive τfValue, this patent is by changing Li2O-3MgO-mTiO2, wherein 4.1≤m≤ 6.TiO in system2Content can improve the ε of materialrValue, the τ for adjusting materialfThe sintering temperature of value and reduction material, so as to Obtain the medium ceramic material of a kind of low cost, low-density and excellent performance.
The content of the invention
The present invention is by changing Li2O-3MgO-mTiO2, wherein 4.1≤m≤6, TiO in system2Content improving material εrValue, the τ for adjusting materialfThe sintering temperature of value and reduction material, so as to obtain a kind of low cost, low-density and performance Excellent temperature-stabilized microwave medium ceramic material.
The chemical constitution formula of microwave dielectric ceramic materials according to the present invention is：Li2O-3MgO-mTiO2, wherein 4.1≤m≤6.
The preparation method of microwave dielectric ceramic materials is concretely comprised the following steps：
(1) with high-purity powder Li of purity >=99%2CO3, MgO and TiO2Li is pressed for raw material2O-3MgO-mTiO2, wherein 4.1 The stoichiometric proportion of≤m≤6 carries out weighing；Afterwards, according to powder, zirconia ball and absolute ethyl alcohol mass ratio be 1：2：1 ratio Example sequentially adds zirconia ball and absolute ethyl alcohol in powder, ball milling 4 hours, it is levigate after the flash baking at 100～120 DEG C, And process of sieving is carried out to powder, the pressed by powder after sieving is into cylindric；Cylinder is placed in alumina crucible carry out it is pre- Burn, calcined temperature is respectively 900 DEG C～950 DEG C, temperature retention time is 4h, and heating rate is 5 DEG C/min.
(2) after the pre-burning that will be obtained in step (1), cylinder carries out preliminary crushing in grinding；Afterwards, according to powder, zirconium oxide Ball is 1 with absolute ethyl alcohol mass ratio：2：During 1 ratio is sequentially placed into nylon tank, ball milling was taken out after 4 hours, was put in baker 100 Drying at～120 DEG C obtains powder；Powder after drying adds 5wt% polyvinyl alcohol to be granulated, afterwards by pressed by powder into diameter It is the cylinder sample of 6mm for 12mm thickness, sample is placed in Muffle furnace 550 DEG C and here are heated to the heating rate of 1 DEG C/min Temperature dumping 4 hours, the cylinder sample of drained glue is sintered 4 hours at 950～1300 DEG C and obtains microwave dielectric ceramic materials.
Microwave-medium ceramics prepared by the present invention, its sintering temperature relatively low (as little as 1050 DEG C), density is less, microwave property It is excellent：Moderate dielectric constant (εr), higher Q × f values and nearlyer zero τfValue, with very big commercial application prospect.
Specific embodiment
Embodiment:
Table 1 lists 18 specific embodiments and its microwave dielectric property of the heterogeneity for constituting the present invention.Its preparation Method as described above, carry out the evaluation of microwave dielectric property with cylindrical dielectric resonator method.
This ceramics can be widely used for the manufacture of the microwave electron components and parts such as various medium substrates, antenna and wave filter, meet The technology of Modern Mobile Communications Systems needs.
Table 1：

Claims (1)

1. a kind of inexpensive, low-density temperature-stabilized microwave medium ceramic material, it is characterised in that the microwave-medium ceramics The chemical constitution formula of material is：Li2O-3MgO-mTiO2, wherein 4.1≤m≤6；
The preparation method of the microwave dielectric ceramic materials is concretely comprised the following steps：
(1) with high-purity powder Li of purity >=99%2CO3, MgO and TiO2Li is pressed for raw material2O-3MgO-mTiO2, wherein 4.1≤m≤ 6 stoichiometric proportion carries out weighing；Afterwards, according to powder, zirconia ball and absolute ethyl alcohol mass ratio be 1：2：1 ratio is to powder Sequentially add zirconia ball and absolute ethyl alcohol in body, ball milling 4 hours, it is levigate after the flash baking at 100～120 DEG C, and to powder Body carries out process of sieving, and the pressed by powder after sieving is into cylindric；Cylinder is placed in alumina crucible carries out pre-burning, pre-burning Temperature is respectively 900 DEG C～950 DEG C, and temperature retention time is 4h, and heating rate is 5 DEG C/min；
(2) after the pre-burning that will be obtained in step (1), cylinder carries out preliminary crushing in grinding；Afterwards, according to powder, zirconium oxide Ball is 1 with absolute ethyl alcohol mass ratio：2：During 1 ratio is sequentially placed into nylon tank, ball milling was taken out after 4 hours, was put in baker Drying at 100～120 DEG C obtains powder；Powder after drying adds 5wt% polyvinyl alcohol to be granulated, afterwards by pressed by powder It is the cylinder sample of 6mm into a diameter of 12mm thickness, sample is placed in Muffle furnace and is heated to the heating rate of 1 DEG C/min 550 DEG C and in this temperature dumping 4 hours, the cylinder sample of drained glue is sintered 4 hours at 950～1300 DEG C and obtains microwave Medium ceramic material.
CN201610969200.7A 2016-11-06 2016-11-06 A kind of temperature-stabilized microwave medium ceramic material and preparation method thereof Active CN106518051B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610969200.7A CN106518051B (en) 2016-11-06 2016-11-06 A kind of temperature-stabilized microwave medium ceramic material and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610969200.7A CN106518051B (en) 2016-11-06 2016-11-06 A kind of temperature-stabilized microwave medium ceramic material and preparation method thereof

Publications (2)

Publication Number Publication Date
CN106518051A true CN106518051A (en) 2017-03-22
CN106518051B CN106518051B (en) 2019-07-23

Family

ID=58326005

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610969200.7A Active CN106518051B (en) 2016-11-06 2016-11-06 A kind of temperature-stabilized microwave medium ceramic material and preparation method thereof

Country Status (1)

Country Link
CN (1) CN106518051B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107311645A (en) * 2017-07-11 2017-11-03 桂林理工大学 A kind of wide sintering warm area Li2MgTiO4The preparation method of microwave dielectric ceramic

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104692795A (en) * 2015-02-09 2015-06-10 陕西师范大学 Ultra-low-loss lithium magnesium titanate microwave dielectric ceramic material and preparation method thereof
CN104844193A (en) * 2015-04-08 2015-08-19 天津大学 Lithium-magnesium-titanium-based microwave dielectric ceramic with high Q value and low temperature sintering realization method thereof
CN105801109A (en) * 2016-04-01 2016-07-27 桂林理工大学 Microwave dielectric ceramic Li2Mg2TiO5 low in loss, stable in temperature and low in dielectric constant

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104692795A (en) * 2015-02-09 2015-06-10 陕西师范大学 Ultra-low-loss lithium magnesium titanate microwave dielectric ceramic material and preparation method thereof
CN104844193A (en) * 2015-04-08 2015-08-19 天津大学 Lithium-magnesium-titanium-based microwave dielectric ceramic with high Q value and low temperature sintering realization method thereof
CN105801109A (en) * 2016-04-01 2016-07-27 桂林理工大学 Microwave dielectric ceramic Li2Mg2TiO5 low in loss, stable in temperature and low in dielectric constant

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
HUANFU ZHOU,ETL: "Processing of low-fired glass-free Li2MgTi3O8 microwave dielectric", 《JOURNAL OF ALLOYS AND COMPOUNDS》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107311645A (en) * 2017-07-11 2017-11-03 桂林理工大学 A kind of wide sintering warm area Li2MgTiO4The preparation method of microwave dielectric ceramic

Also Published As

Publication number Publication date
CN106518051B (en) 2019-07-23

Similar Documents

Publication Publication Date Title
Xiang et al. Low-firing and microwave dielectric properties of Na2YMg2V3O12 ceramic
CN108727022B (en) Ultra-low-loss magnesium lithium niobate system microwave dielectric ceramic material and preparation method thereof
CN108358632B (en) Ultralow-temperature sintered high-Q x f-value microwave dielectric material and preparation method thereof
CN110092655B (en) Barium samarium-titanium series low-loss microwave dielectric ceramic and preparation method thereof
CN111763083B (en) Low-temperature sintered ultralow-loss microwave dielectric ceramic and preparation method and application thereof
CN107117967B (en) Low-temperature sintered composite microwave dielectric ceramic material and preparation method thereof
CN109231967B (en) Bi2O3-B2O3Binary system microwave dielectric ceramic material and preparation method thereof
CN104692795A (en) Ultra-low-loss lithium magnesium titanate microwave dielectric ceramic material and preparation method thereof
CN108147809B (en) Medium-low temperature sintered barium-titanium series microwave dielectric material and preparation method thereof
CN108191426B (en) Medium-temperature sintered high-Q-value microwave dielectric material
CN111943671A (en) Wide-sintering temperature zone low-loss microwave dielectric ceramic and preparation method thereof
CN107244916B (en) Niobate-series low-temperature sintered microwave dielectric ceramic material and preparation method thereof
CN113336539A (en) Microwave dielectric ceramic material, preparation method and application
CN110229004B (en) Low-temperature sintered microwave dielectric ceramic material and preparation method thereof
CN102584208A (en) Low-temperature sinterable microwave dielectric ceramic BiZn2VO4 and preparation method thereof
CN109251028A (en) A kind of low high Q lithium magnesium niobium series microwave dielectric ceramic and preparation method thereof that is situated between
CN105669195A (en) Low-dielectric-constant and high-Q-value microwave dielectric ceramic material and preparation method thereof
CN112851347A (en) Low-temperature sintered low-loss oxyfluoride microwave dielectric ceramic and preparation method thereof
CN107253856A (en) A kind of microwave dielectric material of near-zero resonance frequency temperature coefficient and preparation method thereof
CN102887708B (en) Microwave dielectric ceramic NaCa2(Mg1-xZnx)2V3O12 capable of sintering at low temperature and preparation method
CN106518051A (en) Temperature-stable microwave dielectric ceramic material and preparation method thereof
CN104944937A (en) ZnAl2O4/Li4Ti5O12 microwave dielectric ceramic material and preparation method thereof
CN106866143B (en) Microwave complex phase ceramic AWO4-TiO2 and preparation method thereof
CN106587991B (en) Low-temperature sintered composite microwave dielectric ceramic material and preparation method thereof
CN104710175A (en) Low-dielectric-constant lithium magnesium zirconate microwave dielectric ceramic material and preparation method thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant