CN110282968A - A kind of microwave dielectric ceramic materials and preparation method thereof - Google Patents
A kind of microwave dielectric ceramic materials and preparation method thereof Download PDFInfo
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Abstract
Present invention relates particularly to a kind of simple microwave dielectric ceramic materials of formula and preparation method thereof.Chemical composition are as follows: (1-x) MgTiO3+xCaTiO3+ ywt%Er2O3, wherein 0.03≤x≤0.1,0≤y≤1.The present invention is a kind of inexpensive, simple process microwave-medium ceramics, significantly reduce production cost, improve production efficiency, it is a kind of with middle low-k and the small, temperature coefficient of loss is bordering on zero microwave dielectric ceramic materials, suitable for microwave devices such as dielectric resonator, filter and duplexers, low in raw material price, process route are simple and easy.
Description
Technical field
The invention belongs to electronic information function material and device arts, and in particular to be low dielectric during one kind has
Constant, Qf high and temperature coefficient of resonance frequency τfMicrowave dielectric ceramic materials for the features such as being bordering on zero and preparation method thereof.It can
For making the microwave devices such as dielectric resonator, filter and duplexer.
Background technique
In recent years, due to the rapid development of microwave communication cause, mobile communication, satellite communication, global positioning satellite, indigo plant
Demand of the modern communication technologys such as tooth, WLAN field to miniaturization, the microwave circuit of high performance and microwave device
Increasingly increase.Miniaturization, high stability and the cheap approach for realizing microwave equipment are the integrated of microwave circuit.Traditional gold
Belong to resonant cavity and metal waveguide volume and weight is excessive, limits the development of microwave integrated circuit, and microwave dielectric ceramic can
It solves these problems very well.
Microwave dielectric ceramic materials, which refer to, dielectric material and to be completed one or more applied to being used as in microwave frequency band circuit
The ceramics of function.It is widely used as the microwaves such as resonator, filter, dielectric substrate, dielectric guided wave circuit member in modern communication
Device is the key basic material of modern communication technology.Currently, microwave dielectric ceramic materials have been applied to Portable movable electricity
Words, telstar receiver, military radar etc., it is positive in the process of miniaturization and integration of modern communication tools to play
Increasing effect.
Material is the basis of device, with the development of microwave-medium ceramics device, corresponding Jie for being applied to microwave frequency band
Electroceramics should meet the requirements main as follows: miniaturization of the suitable dielectric constant in favor of device, the Qf of ultrahigh quality factor
Value, nearly zero stable frequency-temperature coefficient.
Magnesium titanate ceramics are a kind of important microwave dielectric ceramic materials, because of its abundant raw material, low in cost, therefore increasingly
It is concerned by people, has become one of most widely used microwave dielectric ceramic materials at present, thermal compensation can be made with it
Capacitor, multilayer ceramic capacitor, dielectric filter and dielectric resonator etc..MgTiO3The temperature coefficient of resonance frequency of ceramics
τ f=-50ppm/ DEG C makes it be bordering on zero to adjust its temperature coefficient of resonance frequency, and people are generally using doping resonance frequency temperature
Spend the CaTiO that coefficient is+800ppm/ DEG C3To obtain the material close to zero temperature coefficient of resonance frequency.MgO-CaO-TiO2
(MCT) system ceramic material is a kind of good microwave dielectric ceramic materials, however, wherein metatitanic acid calcium phase there are dielectric loss compared with
High deficiency is unable to satisfy the requirement of filter with low insertion loss microwave device, MgO-CaO-TiO2The sintering temperature of system ceramic material is
1400~1450 DEG C, because its sintering temperature is higher, so that sintering higher cost, limits the application of MCT system ceramic material.
Therefore, a kind of simple process is currently needed, the cost of raw material is relatively low, sintering temperature is relatively low and at the same time meeting
The microwave-medium ceramics of low loss characteristic, to meet the requirement of microwave communication industry.
Summary of the invention
Have the characteristics that middle low-k, Qf high and rate of temperature change are low the object of the present invention is to provide a kind of
Microwave dielectric ceramic materials and preparation method thereof.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of microwave dielectric ceramic materials, by main crystal phase material and doping phase material through ball milling mixing, pre-burning, doping ball milling, spray
Mist granulation is made.Wherein: the main crystal phase material is MgTiO3Mass percent is 90~97%, CaTiO3Mass percent is 3
~10%；The doping phase material Er2O3, mass percent is 0~1%.
MgTiO in the main crystal phase material3、CaTiO3Between molar ratio be 1-x:x, x be 0.03~0.1.
The doping phase material is oxide Er2O3, mass percent is 0~1%.
A kind of preparation method of microwave dielectric ceramic materials, includes the following steps:
(1), prepared by main crystal phase material, weighs light MgO, TiO respectively in molar ratio2And CaCO3、TiO2, by material: ball: the ratio of water
Example 1:2:0.8 carries out ball milling, and after filters pressing drying, pre-burning at high temperature synthesizes main crystal phase material MgTiO3And CaTiO3。
(2), the main crystal phase material after pre-burning is weighed after crushing by the molar ratio of 1-x:x, adds 0~1% doping phase
Material Er2O3, secondary ball milling is carried out by the condition of step 1, the PVA solution of 22wt% is added in slurry, is spray-dried glomeration
Grain.
Microwave dielectric ceramic materials of the invention at being grouped as are as follows: (1-x) MgTiO3+xCaTiO3+ ywt% Er2O3,
It is 0~1 that wherein x, which is 0.03~0.15, y,.
The crucial group that the present invention forms microwave dielectric ceramic materials becomes (1-x) MgTiO3+xCaTiO3+ ywt% Er2O3,
Contain magnesium, calcium, titanium and er element in formula components, raw material Mg, Ca, Ti, the Er for preparing this microwave dielectric ceramic materials are
Salt and oxide containing these elements.Wherein, doped chemical erbium is the quality factor q in order to adjust microwave dielectric ceramic materials
F reduces sintering temperature.
Primary focus of the invention is the component prescription of microwave dielectric ceramic materials, can basis in actual application
It needs to adjust accordingly synthetic method and production technology, flexibility is big.Solid reaction process, colloidal sol-can be used in synthetic method
Gel method, coprecipitation, the synthetic method of vapour deposition process or other ceramic materials are realized.The present invention, which selects, is suitable for industry greatly
The solid reaction process of production, being conducive to production cost reduces.
The detection of microwave dielectric ceramic materials characteristic of the invention is to use to be pressed into disk, high temperature sintering, burning infiltration silver electricity
Pole measures the characterisitic parameter of tile with HP4291B impedance analyzer.
The characteristic and Heterosis of microwave dielectric ceramic materials of the present invention exist: 1. material composition is simple, raw material
Compare it is abundant, it is environmental-friendly；2. calcined temperature is lower in preparation process, production cost is reduced；3. material is using element erbium as mixing
Miscellaneous element；4. by adjusting metatitanic acid calcium content tunable dielectric constant and rate of temperature change；5. passing through erbium in modifying ingredients composition
Content, adjustable quality factor reduce sintering temperature.
The electrical property of microwave dielectric ceramic materials of the present invention can realize following parameter request: dielectric constant is 20~
22, Qf >=65000GHz, τf≈0±2ppm/℃。
The invention has the beneficial effects that: preparation method simple process, production cost is low, easy to accomplish, and sintering temperature is low,
The Qf value for improving material, reduces the τ of productfValue, the requirement being able to satisfy under microwave condition.
The contents of the present invention are further described with the following Examples.Following embodiment only meets the technology of the present invention
Several examples of content do not illustrate that present invention is limited only to contents described in following examples.The ingredient that focuses on of the invention is matched
Side, the raw material, process and step can be adjusted correspondingly according to actual production conditions, and flexibility is big.
Fig. 1 is the microwave dielectric ceramic materials schematic diagram of internal structure of the present invention observed.
Specific embodiment
The present invention uses light MgO, the CaCO of purity assay3、TiO2Principal crystalline phase is prepared for raw material, is 4N's with purity
Er2O3It is doped, specific embodiment is as follows: weighing ingredient by table 1, mixture is put into stirring-type ball grinder, by pellet
Water quality ratio 1:2:0.8, ball milling 2~6 hours, revolving speed was 260 revs/min.Granularity is controlled in D50Within=1.2 μm, by ball milling
Mixed material filters pressing is put in 100 DEG C of baking oven drying, smashes it through 40 meshes, the pre-burning of table conditional is pressed in chamber type electric resistance furnace,
It is spare to smash it through 40 meshes；In the ratio addition doping phase material Er in table 22O3Secondary ball milling is carried out, granularity is controlled in 0.8 μ
For m hereinafter, the PVA solution of 22wt% is added in slurry, progress mist projection granulating forms outer diameter Φ 12.2mm with handpress 20MPa, thick
Spend the disk of 2mm.Green compact sample is placed in sintering furnace, under the conditions of 1320 DEG C/5H, sinters tile sample, two sides coating silver into
It starches, burning infiltration under the conditions of 850 DEG C/10M is tested for the property sample by HP4291B impedance analyzer.
The specific embodiment of the invention is shown in Table 3 at porcelain density, dielectric properties result in detail.
1 main crystal phase material synthesis condition of table.
2 finished product material list of ingredients of table.
The properties of sample of each example of table 3.
Claims (5)
1. a kind of microwave dielectric ceramic materials, it is characterised in that by main crystal phase material and doping phase material through ball milling mixing, pre-burning,
Doping ball milling, mist projection granulating are made.
2. wherein: the main crystal phase material is MgTiO3Mass percent is 90~97%, CaTiO3Mass percent be 3~
10%；The doping phase material Er2O3, mass percent is 0~1%.
3. the microwave dielectric ceramic materials according to claim 1, which is characterized in that MgTiO in the main crystal phase material3、
CaTiO3Between molar ratio be 1-x:x, x be 0.03~0.1.
4. the microwave dielectric ceramic materials according to claim 1, which is characterized in that the doping phase material is oxide
Er2O3, mass percent is 0~1%.
5. a kind of preparation method of microwave dielectric ceramic materials includes the following steps: prepared by main crystal phase material, distinguishes in molar ratio
Weigh light MgO, TiO2And CaCO3、TiO2, in material: ball: the ratio 1:2:0.8 of water carries out ball milling, after filters pressing drying, in high temperature
Lower pre-burning synthesizes main crystal phase material MgTiO3And CaTiO3；Main crystal phase material after pre-burning is claimed after crushing by the molar ratio of 1-x:x
It takes, adds 0~1% doping phase material Er2O3, secondary ball milling is carried out by the condition of step 1, the PVA of 22wt% is added in slurry
Solution is spray dried to spherical particle.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110746183A (en) * | 2019-11-28 | 2020-02-04 | 无锡鑫圣慧龙纳米陶瓷技术有限公司 | Medium-temperature sintered temperature-stable microwave dielectric ceramic and preparation method thereof |
| CN110922183A (en) * | 2019-11-13 | 2020-03-27 | 深圳顺络电子股份有限公司 | Preparation method of microwave dielectric sintered powder material, microwave dielectric ceramic and application thereof |
| CN111470861A (en) * | 2020-04-22 | 2020-07-31 | 吴坚强 | Microwave dielectric ceramic material and method for preparing microwave ceramic filter device by using same |
| CN112194483A (en) * | 2020-10-23 | 2021-01-08 | 厦门松元电子有限公司 | High-strength calcium-magnesium-titanium microwave dielectric ceramic material and preparation method thereof |
| CN112624755A (en) * | 2020-12-02 | 2021-04-09 | 无锡市高宇晟新材料科技有限公司 | Microwave dielectric ceramic material and preparation method thereof |
| CN114890786A (en) * | 2022-04-18 | 2022-08-12 | 浙江钛迩赛新材料有限公司 | Near-zero temperature drift 5G ceramic filter material and preparation method thereof |
| CN115611625A (en) * | 2022-11-15 | 2023-01-17 | 南京国睿微波器件有限公司 | Magnesium titanate-based microwave dielectric ceramic and preparation process thereof |
| CN116375464A (en) * | 2023-03-27 | 2023-07-04 | 哈尔滨工业大学 | Temperature-stable medium-dielectric-constant microwave dielectric ceramic material and preparation method thereof |
| CN116715517A (en) * | 2023-06-06 | 2023-09-08 | 大富科技(安徽)股份有限公司 | 5G microwave dielectric ceramic material, preparation method thereof and high-frequency communication device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110922183A (en) * | 2019-11-13 | 2020-03-27 | 深圳顺络电子股份有限公司 | Preparation method of microwave dielectric sintered powder material, microwave dielectric ceramic and application thereof |
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| CN111470861A (en) * | 2020-04-22 | 2020-07-31 | 吴坚强 | Microwave dielectric ceramic material and method for preparing microwave ceramic filter device by using same |
| CN111470861B (en) * | 2020-04-22 | 2022-03-01 | 吴坚强 | Microwave dielectric ceramic material and method for preparing microwave ceramic filter device by using same |
| CN112194483A (en) * | 2020-10-23 | 2021-01-08 | 厦门松元电子有限公司 | High-strength calcium-magnesium-titanium microwave dielectric ceramic material and preparation method thereof |
| CN112624755A (en) * | 2020-12-02 | 2021-04-09 | 无锡市高宇晟新材料科技有限公司 | Microwave dielectric ceramic material and preparation method thereof |
| CN114890786A (en) * | 2022-04-18 | 2022-08-12 | 浙江钛迩赛新材料有限公司 | Near-zero temperature drift 5G ceramic filter material and preparation method thereof |
| CN115611625A (en) * | 2022-11-15 | 2023-01-17 | 南京国睿微波器件有限公司 | Magnesium titanate-based microwave dielectric ceramic and preparation process thereof |
| CN116375464A (en) * | 2023-03-27 | 2023-07-04 | 哈尔滨工业大学 | Temperature-stable medium-dielectric-constant microwave dielectric ceramic material and preparation method thereof |
| CN116375464B (en) * | 2023-03-27 | 2024-07-09 | 哈尔滨工业大学 | Temperature-stable medium-dielectric-constant microwave dielectric ceramic material and preparation method thereof |
| CN116715517A (en) * | 2023-06-06 | 2023-09-08 | 大富科技(安徽)股份有限公司 | 5G microwave dielectric ceramic material, preparation method thereof and high-frequency communication device |
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Application publication date: 20190927 |