CN102875129B - Spinel type solid solution medium ceramics materials with magnetic-dielectric functions and preparation method thereof - Google Patents

Spinel type solid solution medium ceramics materials with magnetic-dielectric functions and preparation method thereof Download PDF

Info

Publication number
CN102875129B
CN102875129B CN201210388280.9A CN201210388280A CN102875129B CN 102875129 B CN102875129 B CN 102875129B CN 201210388280 A CN201210388280 A CN 201210388280A CN 102875129 B CN102875129 B CN 102875129B
Authority
CN
China
Prior art keywords
hours
ball milling
preparation
solid solution
spinel
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.)
Active
Application number
CN201210388280.9A
Other languages
Chinese (zh)
Other versions
CN102875129A (en
Inventor
汪宏
何立
周迪
向锋
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.)
Xian Jiaotong University
Original Assignee
Xian Jiaotong University
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 Xian Jiaotong University filed Critical Xian Jiaotong University
Priority to CN201210388280.9A priority Critical patent/CN102875129B/en
Publication of CN102875129A publication Critical patent/CN102875129A/en
Application granted granted Critical
Publication of CN102875129B publication Critical patent/CN102875129B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Compositions Of Oxide Ceramics (AREA)
  • Soft Magnetic Materials (AREA)

Abstract

The invention provides spinel type solid solution medium ceramics materials with magnetic-dielectric functions and a preparation method thereof. On the basis of the structural general formula AB2O4 of spinel, spinel type ferrite ceramics and spinel type microwave dielectric ceramics are selected, solid solution is synthesized at one time by adjusting the raw material ratio of the ferrite to the microwave dielectric ceramics, and a series of the medium ceramics materials which have the magnetic property, an excellent dielectric property and microwave performance are obtained; and the specific structural expression general formula is xA2B4O8-(1-X)Li2MeTi3O8, wherein x is more than or equal to 0.01 and less than or equal to 0.99, A is one or more of Ni<2+>, Cu<2+>, Zn<2+>, Mg<2+>, Fe<3+>, Co<2+>, and Li<+>, B is one or two of Fe<3+> and Co<2+>, and Me is one or more of Zn<2+>, Co<2+>, and Mg<2+>.

Description

A kind of spinel-type solid solution magnetic dielectric function medium ceramic material and preparation method thereof
Technical field
The invention belongs to electronic ceramic and preparation field thereof, particularly a kind of spinel-type solid solution magnetic dielectric function medium ceramic material and preparation method thereof.
Background technology
The fast development of information industry requires the electronics such as communication, radar, navigation, electronic countermeasures to have the characteristics such as multi-functional, miniaturization, high maneuverability energy, this just requires relevant electronic material to have multifunctionality, as magnetic electricity performance, magneto-optical property, flexible piezoelectric etc., wherein magneto-electric behavior receives much concern.As everyone knows, the square root of the electromagnetic wavelength transmitting in dielectric material and the dielectric constant of medium and the product of magnetic permeability is inversely proportional to, therefore adopt the magnetic electric compound material with high dielectric constant and higher magnetic permcability in the situation that not changing device and Antenna Design, greatly to reduce the size of device and antenna.In addition, low-loss magnetic dielectric composite material can be applied to make the devices such as LC oscillator, filter, frequency converter, and the magnetic electric compound material with magnetoelectric effect also can be applicable to transducer, actuator and sensor aspect.
Microwave-medium ceramics is mainly used in making the microwave devices such as resonator, filter, dielectric antenna, medium guided wave loop, can be used for the aspects such as mobile communication, satellite communication and radar.Along with science and technology development with rapid changepl. never-ending changes and improvements, the swift and violent increase of communication information amount, and the requirement of people to radio communication, oneself becomes the inexorable trend of current development communication technologies to use the microwave telecommunication systems such as satellite communication and direct satellite broadcasting TV.Along with electronic information technology is constantly to high frequency and digitlization future development, the miniaturization to components and parts, integrated so that modular requirement is also more and more urgent.
The monophase materials simultaneously with high dielectric constant and higher magnetic permcability is very rare, traditional single-phase ferrite ceramics, as nickel zinc, manganese-zinc ferrite, although there is higher dielectric constant and magnetic permeability under low frequency, but low-frequency dielectric loss is also very large, and in microwave frequency range, their dielectric loss is still higher, is difficult to be widely used in wide frequency range.Nowadays the magnetic electric compound material overwhelming majority receiving much concern is magnetic material and non magnetic dielectric material to be carried out to two-phase or multiphase is compound, to obtain the composite material with magnetic dielectric function.
For ceramic base two-phase is burnt material altogether, they can show higher dielectric constant and higher magnetic permeability conventionally under low frequency, but the high loss feature limits of this class material its application under high-frequency range.For Polymers two-phase composite material, owing to being subject to the restriction of the conditions such as sample mechanical strength, processing technology, the volume fraction of Magnetic Phase ferrite ceramics powder is lower (being no more than 50%) conventionally, thereby cause the feature of low magnetic permeability and the low-k of this composite material.In addition, polymer matrix composite is owing to being subject to the restriction of low melting point polymer basis material, and serviceability temperature is conventionally in 200 ° of C.
In sum, along with Multifunctional nursing material, be widely used in the fields such as the devices such as LC oscillator, resonator, filter, frequency converter and dielectric waveguide, medium substrate, the super material of medium, in order to meet device miniaturization and integrated development need, low-loss magnetic dielectric function dielectric material, with its unique performance advantage, becomes the focus of attention that device exploitation is manufactured gradually.
For composite diphase material, the preparation technology of monophase materials is comparatively simple, has avoided the requirement of two-phase co-fire match.There is no at present a kind of magnetic dielectric function medium ceramic material that has low-frequency high dielectric electric constant and high magnetic permeability and the little loss of microwave concurrently, to meet the demand of information and mechanics of communication high frequency and miniaturization development.Therefore, high-k (ε in searching, preparation r>10), higher magnetic permeability (μ rthe New Magnetic Field Controlled dielectric function medium ceramic material of >5), low-loss (Qf > 5000GHz), near-zero resonance frequency temperature coefficient (TCF=0ppm/ ° of C), low-cost (not containing or contain a small amount of precious metal), environmental protection (at least unleaded, not contain as far as possible or contain less poisonous raw material) becomes the popular direction of current research.
Summary of the invention
First object of the present invention is to provide a kind of spinel-type solid solution magnetic dielectric function medium ceramic material; Second object of the present invention is to provide the preparation method of above-mentioned spinel-type solid solution magnetic dielectric function medium ceramic material.
For achieving the above object, the present invention has adopted following technical scheme.
A spinel-type solid solution magnetic dielectric function medium ceramic material, the structure representation general formula of this magnetic dielectric function medium ceramic material is: xA 2b 4o 8-(1-x) Li 2meTi 3o 8, wherein A is Ni 2+, Cu 2+, Zn 2+, Mg 2+, Co 2+, Fe 3+or Li +in one or more, B is Fe 3+or Co 2+in one or both, Me is Zn 2+, Co 2+or Mg 2+in one or more, 0.01≤x≤0.99.
The preparation method of above-mentioned spinel-type solid solution magnetic dielectric function medium ceramic material, comprises the following steps:
1) by raw material NiO, CuO, ZnO, MgO, Fe 2o 3, Li 2cO 3, TiO 2, Co 2o 3press general formula xA 2b 4o 8-(1-x) Li 2meTi 3o 8preparation, wherein A is Ni 2+, Cu 2+, Zn 2+, Mg 2+, Co 2+, Fe 3+or Li +in one or more, B is Fe 3+or Co 2+in one or both, Me is Zn 2+, Co 2+or Mg 2+in one or more, 0.01≤x≤0.99;
2) raw material after preparation is mixed, ball milling 4 ~ 8 hours, ball milling post-drying, cross 200 mesh sieves, briquetting, then in 700 ~ 1000 ° of C pre-burnings, the temperature retention time of pre-burning is 4 ~ 6 hours;
3) after pre-burning, carry out secondary ball milling, 5 ~ 6 hours post-dryings of ball milling, granulation, then sieve and obtain porcelain through 60 orders and 120 eye mesh screen bilayers, porcelain is compressing after under 900 ~ 1350 ° of C sintering 2 ~ 4 hours.
The temperature of described oven dry is 100 ~ 200 ° of C.
The preparation method of above-mentioned spinel-type solid solution magnetic dielectric function medium ceramic material, comprises the following steps:
1) by raw material Li 2cO 3, TiO 2, ZnO and Fe 2o 3press general formula xLiFe 5o 8-(1-x) Li 2znTi 3o 8preparation, 0.01≤x≤0.99;
2) raw material after preparation is mixed, ball milling 4 hours, ball milling post-drying, cross 200 mesh sieves, briquetting, then in 900 ° of C pre-burnings, the temperature retention time of pre-burning is 4 hours;
3) after pre-burning, carry out secondary ball milling, 5 hours post-dryings of ball milling, granulation, then sieve and obtain porcelain through 60 orders and 120 eye mesh screen bilayers, porcelain is compressing after under 1025 ~ 1125 ° of C sintering 2 ~ 3 hours.
The preparation method of above-mentioned spinel-type solid solution magnetic dielectric function medium ceramic material, comprises the following steps:
1) by raw material Li 2cO 3, TiO 2, MgO and Fe 2o 3press general formula 0.5LiFe 5o 8-0.5Li 2mgTi 3o 8preparation;
2) raw material after preparation is mixed, ball milling 4 hours, ball milling post-drying, cross 200 mesh sieves, briquetting, then in 900 ° of C pre-burnings, the temperature retention time of pre-burning is 4 hours;
3) after pre-burning, carry out secondary ball milling, 5 hours post-dryings of ball milling, granulation, then sieve and obtain porcelain through 60 orders and 120 eye mesh screen bilayers, porcelain is compressing after under 1025 ~ 1125 ° of C sintering 2 ~ 3 hours.
The preparation method of above-mentioned spinel-type solid solution magnetic dielectric function medium ceramic material, comprises the following steps:
1) by raw material Li 2cO 3, TiO 2, ZnO, NiO, CuO and Fe 2o 3press general formula 0.25Ni 0.8cu1 2fe 4o 8-0.75Li 2znTi 3o 8preparation;
2) raw material after preparation is mixed, ball milling 4 hours, ball milling post-drying, cross 200 mesh sieves, briquetting, then in 700 ~ 800 ° of C pre-burnings, the temperature retention time of pre-burning is 4 hours;
3) after pre-burning, carry out secondary ball milling, 5 hours post-dryings of ball milling, granulation, then sieve and obtain porcelain through 60 orders and 120 eye mesh screen bilayers, porcelain is compressing after under 900~1000 ° of C sintering 2 ~ 3 hours.
The preparation method of above-mentioned spinel-type solid solution magnetic dielectric function medium ceramic material, comprises the following steps:
1) by raw material Li 2cO 3, TiO 2, ZnO, Co 2o 3and Fe 2o 3press general formula 0.25LiFe 3co 2o 8-0.75Li 2znTi 3o 8preparation;
2) raw material after preparation is mixed, ball milling 4 hours, ball milling post-drying, cross 200 mesh sieves, briquetting, then in 900 ° of C pre-burnings, the temperature retention time of pre-burning is 4 hours;
3) after pre-burning, carry out secondary ball milling, 5 hours post-dryings of ball milling, granulation, then sieve and obtain porcelain through 60 orders and 120 eye mesh screen bilayers, porcelain is compressing after under 1025~1125 ° of C sintering 2 ~ 3 hours.
The present invention adopts the method for solid phase reaction sintering to prepare above-mentioned ceramic material.First according to formula, choose initial oxide and substituent (carbonate), then by a ball milling, oxide is mixed, then by presintering process, make oxide carry out preliminary reaction, by the particle size of secondary ball milling refinement reactant, finally by sintering process, obtain needed ceramics sample again.By a kind of so simple preparation method, the dielectric constant of the ceramics sample obtaining changes between 10 ~ 30 with composition, and magnetic permeability is at 5 ~ 40(≤100MHz) between change, Qf is distributed in 1000 ~ 20000GHz, sintering temperature is 900 ~ 1350 ° of C.
The prepared spinel-type solid solution magnetic dielectric function medium ceramic material of the present invention has following characteristics: low frequency relative permeability is 5 ~ 40(≤100MHz), low-frequency dielectric constant is 10 ~ 40(≤100MHz), there is lower low-frequency dielectric loss (tan δ <10 -2, 100MHz), microwave permittivity is 10 ~ 30(7GHz), have good microwave property, quality factor q f=1000 ~ 20000GHz, the sintering temperature of this ceramic material is 900 ~ 1350 ° of C in addition, and chemical composition and preparation technology are simple, and thing is mutually single.
Accompanying drawing explanation
Fig. 1 is 0.25LiFe described in embodiment 2 5o 8-0.75Li 2znTi 3o 8ceramic material ESEM microphoto, 1050 ° of C sintering 2 hours.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
The structure representation general formula of spinel-type solid solution magnetic dielectric function medium ceramic material of the present invention is: xA 2b 4o 8-(1-x) Li 2meTi 3o 8, wherein A is Ni 2+, Cu 2+, Zn 2+, Mg 2+, Co 2+, Fe 3+or Li +in one or more, B is Fe 3+or Co 2+in one or both, Me is Zn 2+, Co 2+or Mg 2+in one or more, 0.01≤x≤0.99.
The concrete preparation process of spinel-type solid solution magnetic dielectric function medium ceramic material of the present invention is:
1) by chemical raw material NiO, CuO, ZnO, MgO, Fe 2o 3, Li 2cO 3, TiO 2, Co 2o 3by formula general formula xA 2b 4o 8-(1-x) Li 2meTi 3o 8preparation, wherein A is Ni 2+, Cu 2+, Zn 2+, Mg 2+, Co 2+, Fe 3+or Li +in one or more, B is Fe 3+or Co 2+in one or both, Me is Zn 2+, Co 2+or Mg 2+in one or more, 0.01≤x≤0.99;
2) chemical raw material after preparation is mixed, then put into nylon tank, to the absolute ethyl alcohol adding in nylon tank with the weight such as raw material, ball milling 4 ~ 8 hours, is fully mixed and finely ground, and after ball milling, takes out, then in 100 ~ 200 ° of C flash bakings, after drying, cross 200 mesh sieves, be then pressed in advance block;
3) by obtaining sample after block pre-burning, burn piece, the condition of pre-burning is 700 ~ 1000 ° of C insulations 4 ~ 6 hours;
4) sample is burnt to piece and pulverize rear ball milling 5 ~ 6 hours, fully be mixed and finely ground, after ball milling, in 100 ~ 200 ° of C, dry, after oven dry, add (8 ~ 15%) PVA adhesive (5% polyvinyl alcohol water solution) granulation, then with 60 orders and 120 eye mesh screen bilayers, sieve successively, obtain granulation porcelain powder;
5) granulation porcelain powder is compressing on demand, by hydraulic press (YE-600 Jinan testing machine factory), be pressed into block, pressure size used is 150 ~ 180Mpa/m 2then under 900 ~ 1350 ° of C, sintering becomes porcelain in 2 ~ 4 hours, can obtain spinel-type solid solution magnetic dielectric function medium ceramic material.
Main feature of the present invention is to using spinel-type high magnetic conductivity ferrite material and spinel-type microwave dielectric material as pivot, make the two generate the solid solution dissolving each other with arbitrary proportion, retain the microwave dielectric property of ferritic magnetic performance and microwave dielectric material simultaneously.The present invention is theoretical according to morphology and dielectric, with AB 2o 4this typical spinelle consists of basis, uses Zn 2+, Co 2+, Mg 2+, Li +, Fe 3+in the combination of one or more ions occupy A position, use Fe 3+, Mg 2+, Li +, Co 2+, Ti 4+, Ni 2+, Cu 2+in one or more ions occupy B position, do not adding under the prerequisite of any sintering aid, can in the temperature range of 900 ° of C~1350 ° C, go out new function pottery fine and close and that simultaneously have higher magnetic permeability, high dielectric constant and good microwave dielectric property by sintering, this class pottery can be used as the dielectric materials such as radio frequency multilayer ceramic capacitor, chip microwave dielectric resonator or filter, ceramic antenna, multi-chip module (MCM) and uses.
Embodiment 1:
By analytically pure raw material Li 2cO 3, TiO 2, ZnO and Fe 2o 3by formula 0.5LiFe 5o 8-0.5Li 2znTi 3o 8preparation.After preparation, abundant mixing and ball milling is 4 hours, then dry, sieve, briquetting, briquetting was by 900 ° of C pre-burnings 4 hours, then after the bulk sample after pre-burning being pulverized, carry out again secondary ball milling 5 hours, levigate post-drying, granulation, then through 60 orders and 120 eye mesh screen bilayers, sieve, can obtain required porcelain.By porcelain compressing (sheet or column) on demand, then under 1025 ~ 1125 ° of C air, sintering 2 ~ 3h becomes porcelain, can obtain spinel-type solid solution magnetic dielectric function medium ceramic material.
The performance of this group ceramic material reaches following index:
At 2 hours resulting samples of 1050 ℃ of sintering, in 1MHz ~ 100MHz frequency range, have: relative permeability μ r=45 ~ 15, relative dielectric constant ε r=20 ~ 19.5, dielectric loss tan δ=2 * 10 -2~ 5 * 10 -3, the dielectric property ε under microwave r=19.0(7.0GHz), quality factor q=710, Qf=5000GHz.
Embodiment 2:
By analytically pure raw material Li 2CO 3, TiO 2, ZnO and Fe 2o 3by formula 0.25LiFe 5o 8-0.75Li 2znTi 3o 8(also can be written as [(Zn 0.375fe 0.625) (Li 0.875ti 1.125)] O 4) preparation.After preparation, abundant mixing and ball milling is 4 hours, then dry, sieve, briquetting, briquetting was by 900 ° of C pre-burnings 4 hours, then after the bulk sample after pre-burning being pulverized, carry out again secondary ball milling 5 hours, levigate post-drying, granulation, then through 60 orders and 120 eye mesh screen bilayers, sieve, can obtain required porcelain.By porcelain compressing (sheet or column) on demand, then under 1025 ~ 1125 ° of C air, sintering 2 ~ 3h becomes porcelain, can obtain spinel-type solid solution magnetic dielectric function medium ceramic material, referring to Fig. 1.
The performance of this group ceramic material reaches following index:
At 2 hours resulting samples of 1050 ℃ of sintering, in 1MHz ~ 10MHz frequency range, have: relative permeability μ r=38.2 ~ 15, relative dielectric constant ε r=19.6 ~ 19.3, dielectric loss tan δ=8 * 10 -3~ 2 * 10 -3, the DIELECTRIC CONSTANT ε under microwave r=19.0(6.84GHz), quality factor q=1720, Qf=11700GHz, the temperature coefficient of resonance frequency TCF=-62ppm/ ° C(25 ~ 85 ° C under microwave).
Embodiment 3:
By analytically pure raw material Li 2cO 3, TiO 2, ZnO and Fe 2o 3by formula 0.23LiFe 5o 8-0.77Li 2znTi 3o 8preparation.After preparation, abundant mixing and ball milling is 4 hours, then dry, sieve, briquetting, briquetting was by 900 ° of C pre-burnings 4 hours, then after the bulk sample after pre-burning being pulverized, carry out again secondary ball milling 5 hours, levigate post-drying, granulation, then through 60 orders and 120 eye mesh screen bilayers, sieve, can obtain required porcelain.By porcelain compressing (sheet or column) on demand, then under 1025 ~ 1125 ° of C air, sintering 2 ~ 3h becomes porcelain, can obtain spinel-type solid solution magnetic dielectric function medium ceramic material.
The performance of this group ceramic material reaches following index:
At 2 hours resulting samples of 1050 ℃ of sintering, in 1MHz ~ 10MHz frequency range, have: relative permeability μ r=18.6 ~ 10, relative dielectric constant ε r=19.6 ~ 19.4, dielectric loss tan δ=5 * 10 -3~ 8 * 10 -4, the dielectric property ε under microwave r=19.2(6.8GHz), quality factor q=2058, Qf=14000GHz, the temperature coefficient of resonance frequency TCF=-60ppm/ ° C(25 ° C ~ 85 ° C under microwave).
Embodiment 4:
By analytically pure raw material Li 2cO 3, TiO 2, ZnO and Fe 2o 3by formula 0.24LiFe 5o 8-0.76Li 2znTi 3o 8preparation.After preparation, abundant mixing and ball milling is 4 hours, then dry, sieve, briquetting, briquetting was by 900 ° of C pre-burnings 4 hours, then after the bulk sample after pre-burning being pulverized, carry out again secondary ball milling 5 hours, levigate post-drying, granulation, then through 60 orders and 120 eye mesh screen bilayers, sieve, can obtain required porcelain.By porcelain compressing (sheet or column) on demand, then under 1025 ~ 1125 ° of C air, sintering 2 ~ 3h becomes porcelain, can obtain spinel-type solid solution magnetic dielectric function medium ceramic material.
The performance of this group ceramic material reaches following index:
At 2 hours resulting samples of 1050 ℃ of sintering, in 1MHz~10MHz frequency range, have: relative permeability μ r=25.1 ~ 12, relative dielectric constant ε r=19.8 ~ 19.4, dielectric loss tan δ=8 * 10 -31 * 10 -3, the dielectric property ε under microwave r=19.3(6.9GHz), quality factor q=1800, Qf=12400GHz.
Embodiment 5:
By analytically pure raw material Li 2cO 3, TiO 2, MgO and Fe 2o 3by formula 0.5LiFe 5o 8-0.5Li 2mgTi 3o 8preparation.After preparation, abundant mixing and ball milling is 4 hours, then dry, sieve, briquetting, briquetting was by 900 ° of C pre-burnings 4 hours, then after the bulk sample after pre-burning being pulverized, carry out again secondary ball milling 5 hours, levigate post-drying, granulation, then through 60 orders and 120 eye mesh screen bilayers, sieve, can obtain required porcelain.By porcelain compressing (sheet or column) on demand, then under 1025 ~ 1125 ° of C air, sintering 2 ~ 3h becomes porcelain, can obtain spinel-type solid solution magnetic dielectric function medium ceramic material.
The performance of this group ceramic material reaches following index:
At 2 hours resulting samples of 1050 ℃ of sintering, in 1MHz ~ 100MHz frequency range, have: relative permeability μ r=15 ~ 5, relative dielectric constant ε r=18.5 ~ 17.5, dielectric loss tan δ=2 * 10 -2~ 8 * 10 -3, the dielectric property ε under microwave r=17.0(7.8GHz), quality factor q=1105, Qf=8608GHz.
Embodiment 6:
By analytically pure raw material Li 2cO 3, TiO 2, ZnO, NiO, CuO and Fe 2o 3by formula 0.25Ni 0.8cu 1.2fe 4o 8-0.75Li 2znTi 3o 8preparation.After preparation, abundant mixing and ball milling is 4 hours, then dry, sieve, briquetting, briquetting was by 700 ~ 800 ° of C pre-burnings 4 hours, then after the bulk sample after pre-burning being pulverized, carry out again secondary ball milling 5 hours, levigate post-drying, granulation, then through 60 orders and 120 eye mesh screen bilayers, sieve, can obtain required porcelain.By porcelain compressing (sheet or column) on demand, then under 900 ~ 1000 ° of C air, sintering 2 ~ 3h becomes porcelain, can obtain spinel-type solid solution magnetic dielectric function medium ceramic material.
The performance of this group ceramic material reaches following index:
At 2 hours resulting samples of 950 ℃ of sintering, in 1MHz ~ 10MHz frequency range, have: relative permeability μ r=20 ~ 8, relative dielectric constant ε r=19.6 ~ 19.4, dielectric loss tan δ=5 * 10 -2~ 8 * 10 -3, the dielectric property ε under microwave r=17.0(7.0GHz), quality factor q=610, Qf=4300GHz.
Embodiment 7:
By analytically pure raw material Li 2cO 3, TiO 2, ZnO, Co 2o 3and Fe 2o 3by formula 0.25LiFe 3co 2o 8-0.75Li 2znTi 3o 8preparation.After preparation, abundant mixing and ball milling is 4 hours, then dry, sieve, briquetting, briquetting was by 900 ° of C pre-burnings 4 hours, then after the bulk sample after pre-burning being pulverized, carry out again secondary ball milling 5 hours, levigate post-drying, granulation, then through 60 orders and 120 eye mesh screen bilayers, sieve, can obtain required porcelain.By porcelain compressing (sheet or column) on demand, then under 1025 ~ 1125 ° of C air, sintering 2 ~ 3h becomes porcelain, can obtain spinel-type solid solution magnetic dielectric function medium ceramic material.
The performance of this group ceramic material reaches following index:
At 2 hours resulting samples of 1075 ℃ of sintering, in 1MHz ~ 100MHz frequency range, have: relative permeability μ r=7.5 ~ 5.5, relative dielectric constant ε r=19.5 ~ 19.2, dielectric loss tan δ=8 * 10 -3~ 3 * 10 -3, the dielectric property ε under microwave r=18.8(6.99GHz), quality factor q=1570, Qf=11000GHz.
It is pointed out that, according to technical scheme of the present invention, above-described embodiment can also be enumerated many, the results show a large amount of according to applicant, in scope proposed by the invention, all can reach object of the present invention.

Claims (5)

1. a spinel-type solid solution magnetic dielectric function medium ceramic material, is characterized in that, is to using spinel-type high magnetic conductivity ferrite material and spinel-type microwave dielectric material as pivot, makes the two generate the mutually single AB of thing dissolving each other with arbitrary proportion 2o 4spinel structure solid solution retains the microwave dielectric property of ferritic magnetic performance and microwave dielectric material simultaneously;
This solid solution structure representation general formula be: xA 2b 4o 8-(1-x) Li 2meTi 3o 8, wherein A is Ni 2+, Cu 2+, Zn 2+, Mg 2+, Co 2+, Fe 3+or Li +in one or more, B is Fe 3+or B is Fe 3+and Co 2+, Me is Zn 2+, Co 2+or Mg 2+in one or more, 0.01≤x≤0.99;
For above-mentioned this kind of AB 2o 4spinel structure solid solution ceramic, in forming the process of solid solution, conventionally by Zn 2+, Co 2+, Mg 2+, Li +, Fe 3+in the combination of one or more ions occupy A position, use Fe 3+, Mg 2+, Li +, Co 2+, Ti 4+, Ni 2+, Cu 2+in one or more ions occupy B position.
2. prepare a method for spinel-type solid solution magnetic dielectric function medium ceramic material as claimed in claim 1, it is characterized in that, comprise the following steps:
1) by raw material NiO, CuO, ZnO, MgO, Fe 2o 3, Li 2cO 3, TiO 2, Co 2o 3press general formula xA 2b 4o 8-(1-x) Li 2meTi 3o 8preparation, wherein A is Ni 2+, Cu 2+, Zn 2+, Mg 2+, Co 2+, Fe 3+or Li +in one or more, B is Fe 3+or B is Fe 3+and Co 2+, Me is Zn 2+, Co 2+or Mg 2+in one or more, 0.01≤x≤0.99;
2) raw material after preparation is mixed, ball milling 4~8 hours, ball milling post-drying, cross 200 mesh sieves, briquetting, then in 700~1000 ℃ of pre-burnings, the temperature retention time of pre-burning is 4~6 hours;
3) after pre-burning, carry out secondary ball milling, 5~6 hours post-dryings of ball milling, granulation, then sieve and obtain porcelain through 60 orders and 120 eye mesh screen bilayers, porcelain is compressing after at 900~1350 ℃ sintering 2~4 hours.
3. prepare a method for spinel-type solid solution magnetic dielectric function medium ceramic material as claimed in claim 1, it is characterized in that, comprise the following steps:
1) by raw material Li 2cO 3, TiO 2, ZnO and Fe 2o 3press general formula xLiFe 5o 8-(1-x) Li 2znTi 3o 8preparation, 0.01≤x≤0.99;
2) raw material after preparation is mixed, ball milling 4 hours, ball milling post-drying, cross 200 mesh sieves, briquetting, then in 900 ℃ of pre-burnings, the temperature retention time of pre-burning is 4 hours;
3) after pre-burning, carry out secondary ball milling, 5 hours post-dryings of ball milling, granulation, then sieve and obtain porcelain through 60 orders and 120 eye mesh screen bilayers, porcelain is compressing after at 1025~1125 ℃ sintering 2~3 hours.
4. prepare a method for spinel-type solid solution magnetic dielectric function medium ceramic material as claimed in claim 1, it is characterized in that, comprise the following steps:
1) by raw material Li 2cO 3, TiO 2, MgO and Fe 2o 3press general formula 0.5LiFe 5o 8-0.5Li 2mgTi 3o 8preparation;
2) raw material after preparation is mixed, ball milling 4 hours, ball milling post-drying, cross 200 mesh sieves, briquetting, then in 900 ℃ of pre-burnings, the temperature retention time of pre-burning is 4 hours;
3) after pre-burning, carry out secondary ball milling, 5 hours post-dryings of ball milling, granulation, then sieve and obtain porcelain through 60 orders and 120 eye mesh screen bilayers, porcelain is compressing after at 1025~1125 ℃ sintering 2~3 hours.
5. prepare a method for spinel-type solid solution magnetic dielectric function medium ceramic material as claimed in claim 1, it is characterized in that, comprise the following steps:
1) by raw material Li 2cO 3, TiO 2, ZnO, NiO, CuO and Fe 2o 3press general formula 0.25Ni 0.8cu 1.2fe 4o 8-0.75Li 2znTi 3o 8preparation;
2) raw material after preparation is mixed, ball milling 4 hours, ball milling post-drying, cross 200 mesh sieves, briquetting, then in 700~800 ℃ of pre-burnings, the temperature retention time of pre-burning is 4 hours;
3) after pre-burning, carry out secondary ball milling, 5 hours post-dryings of ball milling, granulation, then sieve and obtain porcelain through 60 orders and 120 eye mesh screen bilayers, porcelain is compressing after at 900~1000 ℃ sintering 2~3 hours.
CN201210388280.9A 2012-10-12 2012-10-12 Spinel type solid solution medium ceramics materials with magnetic-dielectric functions and preparation method thereof Active CN102875129B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201210388280.9A CN102875129B (en) 2012-10-12 2012-10-12 Spinel type solid solution medium ceramics materials with magnetic-dielectric functions and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201210388280.9A CN102875129B (en) 2012-10-12 2012-10-12 Spinel type solid solution medium ceramics materials with magnetic-dielectric functions and preparation method thereof

Publications (2)

Publication Number Publication Date
CN102875129A CN102875129A (en) 2013-01-16
CN102875129B true CN102875129B (en) 2014-12-10

Family

ID=47476693

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201210388280.9A Active CN102875129B (en) 2012-10-12 2012-10-12 Spinel type solid solution medium ceramics materials with magnetic-dielectric functions and preparation method thereof

Country Status (1)

Country Link
CN (1) CN102875129B (en)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104944947B (en) * 2015-05-20 2017-07-11 电子科技大学 A kind of microwave gyromagnet dielectric composite ceramic material and preparation method thereof
CN112537956B (en) * 2019-09-23 2023-03-28 比亚迪股份有限公司 Black zirconia ceramic and preparation method and application thereof
CN111018509A (en) * 2019-10-30 2020-04-17 北京信息科技大学 Novel ferroelectric semiconductor solid electrolyte material and preparation method and application thereof
CN112538253A (en) * 2020-12-07 2021-03-23 陕西生益科技有限公司 Magnetic dielectric resin composition, laminated board containing same and printed circuit board containing laminated board

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101786875A (en) * 2010-01-02 2010-07-28 桂林理工大学 Microwave medium ceramic material with low-temperature sintering spinel structure and preparation method thereof
JP2011515012A (en) * 2008-12-02 2011-05-12 コカン カンパニー リミテッド Core-shell type negative electrode active material for lithium secondary battery, method for producing the same, negative electrode for lithium secondary battery including the same, and lithium secondary battery
CN102320825A (en) * 2011-08-16 2012-01-18 广西新未来信息产业股份有限公司 Low-temperature sintered microwave dielectric ceramic and sintering method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2011515012A (en) * 2008-12-02 2011-05-12 コカン カンパニー リミテッド Core-shell type negative electrode active material for lithium secondary battery, method for producing the same, negative electrode for lithium secondary battery including the same, and lithium secondary battery
CN101786875A (en) * 2010-01-02 2010-07-28 桂林理工大学 Microwave medium ceramic material with low-temperature sintering spinel structure and preparation method thereof
CN102320825A (en) * 2011-08-16 2012-01-18 广西新未来信息产业股份有限公司 Low-temperature sintered microwave dielectric ceramic and sintering method thereof

Also Published As

Publication number Publication date
CN102875129A (en) 2013-01-16

Similar Documents

Publication Publication Date Title
CN101870584B (en) Preparation method of molybdenum-based ultralow-temperature sintering microwave medium ceramic materials
CN102249663B (en) Bismuth-vanadium-based low temperature sintered microwave dielectric ceramic material and preparation method thereof
CN100591641C (en) Low-temperature sintering Ti-base microwave medium ceramic material and preparation thereof
CN101823880B (en) Phenacite type molybdenum-based and tungsten-based ultralow temperature sintered microwave dielectric ceramic materials and preparation method thereof
CN103204680B (en) Niobate microwave dielectric ceramic LiMNb3O9 and preparation method thereof
CN102875129B (en) Spinel type solid solution medium ceramics materials with magnetic-dielectric functions and preparation method thereof
CN103058657A (en) Microwave dielectric ceramics doped with cobalt oxide and niobium zinc titanate
CN101823879A (en) Scheelite type molybdenum-based ultralow temperature-sintered microwave dielectric ceramic material and preparation method thereof
CN102850051B (en) YFeO3 base bi-phase magnetoelectricity composite material and preparation method thereof
CN104387057B (en) A kind of temperature-stable titanio spinelle microwave-medium ceramics and low temperature preparation method thereof
CN108424134B (en) Garnet type solid solution magneto-dielectric functional dielectric ceramic material and preparation method thereof
CN103214243A (en) Niobium zinc titanate microwave dielectric ceramic and preparation method thereof
CN103467093A (en) Nickel oxide-doped niobium zinc titanate microwave dielectric ceramic and preparation method thereof
CN104744041A (en) Temperature stable type microwave dielectric ceramic Li2Cu2Nb8O23 with low dielectric constant
CN104311008A (en) Temperature-stable medium-dielectric constant microwave dielectric ceramic BaNb4V2O16 and preparation method thereof
CN104710175B (en) A kind of low-k magnesium zirconate lithium microwave dielectric ceramic materials and preparation method thereof
CN101792319B (en) Preparation method of low temperature sintered magnetoelectric composite ceramic material
CN100534949C (en) Yttrium niobate solid-phase reaction synthetic sintering method capable of being used for microwave dielectric ceramic
CN104710176A (en) Ultra-low temperature vanadium-based microwave medium ceramic material stable in sintering temperature and preparation method thereof
CN101265097B (en) Low-temperature sintering composite microwave medium ceramic and preparation method thereof
CN103058658A (en) BaCu(B2O5) doped zinc niobate-titanate microwave dielectric ceramic
CN102351537A (en) High-permittivity microwave medium ceramic material
CN105314976A (en) Ti-based low loss K value microwave dielectric ceramic and preparation method thereof
CN105732031A (en) Nickel-doped Li3Mg2NbO6 ceramic material and preparation method thereof
CN101747055B (en) Low-temperature sintered magnetoelectric composite medium thick film material and preparation method thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant