CN106518051B - A kind of temperature-stabilized microwave medium ceramic material and preparation method thereof - Google Patents

A kind of temperature-stabilized microwave medium ceramic material and preparation method thereof Download PDF

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CN106518051B
CN106518051B CN201610969200.7A CN201610969200A CN106518051B CN 106518051 B CN106518051 B CN 106518051B CN 201610969200 A CN201610969200 A CN 201610969200A CN 106518051 B CN106518051 B CN 106518051B
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CN106518051A (en
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周焕福
谭祥虎
黄瑾
陈秀丽
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Guilin University of Technology
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    • 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
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Abstract

The invention discloses a kind of low costs, the temperature-stabilized microwave medium ceramic material of low-density and preparation method thereof.The chemical constitution formula of the microwave dielectric ceramic materials are as follows: Li2O‑3MgO‑mTiO2(4.1≤m≤6).First by the high-purity powder Li of purity >=99%2CO3, MgO and TiO2By Li2O‑3MgO‑mTiO2The stoichiometric ratio of (4.1≤m≤6) carries out weighing；Again by step (1) raw material wet ball-milling mixing 4h, it is dry after the pre-burning 4h at 900~950 DEG C respectively；After the powder after pre-burning is finally carried out secondary ball milling, addition 5wt% polyvinyl alcohol is granulated, and compression moulding after granulation will be finally sintered 4 hours at 950~1300 DEG C after green body dumping.Microwave-medium ceramics prepared by the present invention have moderate dielectric constant, higher Q × f value and nearlyr zero τfValue has very big commercial application prospect.

Description

A kind of temperature-stabilized microwave medium ceramic material and preparation method thereof
Technical field
The invention belongs to electronic ceramics and its manufacturing field, it is related to resonator, filter, the medium used in microwave frequency band The preparation method of the dielectric ceramic material of the microwave devices such as antenna, dielectric guided wave circuit.
Background technique
Microwave dielectric material refer to applied in microwave frequency band (300MHz~300GHz) circuit be used as medium and complete one The ceramics of kind or multiple functions, mainly for the preparation of the microwaves member device such as resonator, filter, diectric antenna, dielectric guided wave circuit Part.In recent years, as microwave device constantly develops to cost effective, miniaturization and lightweight direction, it is desirable that microwave-medium Material must have excellent microwave dielectric property (high Q × f value, moderate dielectric constant, nearly zero τfValue), low production Cost, low density.Although commercial microwave dielectric ceramic materials have excellent performance at present, such as Ba (Zn1/3Nb2/3)O3, Ba(Mg1/3Nb2/3)O3, Ba (Y1/2Ta1/2)O3, but high sintering temperature and density, expensive raw materials for production limit it in quotient Further applying in industry.Therefore, the raw materials for production of low price is selected to prepare the microwave-medium material of low cost, sintering temperature and low Material has been trend of the times.But the difficulty for finding the material for meeting the above standard is very big, so some researcher Low cost is found in the excellent material system of existing microwave dielectric property, the material of low-density carries out cooling and handles to reach Purpose.The most common method for reducing sintering temperature mainly has following three kinds: (1) adding sintering aid；(2) using ultra-fine Powder；(3) raw material of low melting point is used.But add sintering aid will severe exacerbation material performance, use superfine powder Production cost will be increased, so research direction is concentrated on the raw material using low melting point to realize low-temperature sintering by Many researchers On.
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), which limits it, commercially extensive and persistence answers 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 materialfValue and the sintering temperature for reducing material, thus Obtain a kind of inexpensive, low-density and the medium ceramic material haveing excellent performance.
Summary of the invention
The present invention is by changing Li2O-3MgO-mTiO2, wherein 4.1≤m≤6, TiO in system2Content to improve material εrValue, the τ for adjusting materialfValue and the sintering temperature for reducing material, 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 of the present invention are as follows: Li2O-3MgO-mTiO2, wherein 4.1≤m ≤6。
The preparation method specific steps of microwave dielectric ceramic materials are as follows:
(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 ratio of≤m≤6 carries out weighing；Later, the ratio for being 1:2:1 according to powder, zirconia ball and dehydrated alcohol mass ratio Example sequentially adds zirconia ball and dehydrated alcohol into powder, ball milling 4 hours, it is levigate after the flash baking at 100~120 DEG C, And sieving processing is carried out to powder, the pressed by powder after sieving is at cylindric；Cylindrical body is placed in alumina crucible and is carried out in advance It burns, calcined temperature is respectively 900 DEG C~950 DEG C, soaking time 4h, and heating rate is 5 DEG C/min.
(2) cylindrical body after pre-burning obtained in step (1) is tentatively crushed in grinding；Later, according to powder, oxygen The ratio that change zirconium ball and dehydrated alcohol mass ratio are 1:2:1 is sequentially placed into ball milling in nylon tank and takes out after 4 hours, is put into baker The interior drying at 100~120 DEG C obtains powder；Powder after drying is added 5wt% polyvinyl alcohol and is granulated, later by powder Being pressed into diameter is cylinder sample of the 12mm with a thickness of 6mm, and sample is placed in Muffle furnace and is heated with the heating rate of 1 DEG C/min To 550 DEG C and at this temperature dumping 4 hours, the cylinder sample of drained glue is sintered at 950~1300 DEG C 4 hours i.e. obtain it is micro- Wave medium ceramic material.
Microwave-medium ceramics prepared by the present invention, sintering temperature is lower (down to 1050 DEG C), and density is smaller, microwave property It is excellent: moderate dielectric constant (εr), higher Q × f value and nearlyr zero τfValue has very big commercial application prospect.
Specific embodiment
Embodiment:
Table 1 lists 18 specific embodiments and its microwave dielectric property for constituting heterogeneity of the invention.It is prepared Method is 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 electrons component such as various medium substrates, antenna and filter, meet The technology of Modern Mobile Communications Systems needs.
Table 1:

Claims (1)

1. the temperature-stabilized microwave medium ceramic material of a kind of low cost, low-density, it is characterised in that the microwave-medium ceramics The chemical constitution formula of material are as follows: Li2O-3MgO-mTiO2, wherein 4.1≤m≤6；
The preparation method specific steps of the microwave dielectric ceramic materials are as follows:
(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 ratio carries out weighing；Later, according to the ratio that powder, zirconia ball and dehydrated alcohol mass ratio are 1:2:1 to powder Sequentially add zirconia ball and dehydrated 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 sieving processing, and the pressed by powder after sieving is at cylindric；Cylindrical body is placed in alumina crucible and carries out pre-burning, pre-burning Temperature is respectively 900 DEG C~950 DEG C, soaking time 4h, and heating rate is 5 DEG C/min；
(2) cylindrical body after pre-burning obtained in step (1) is tentatively crushed in grinding；Later, according to powder, zirconium oxide The ratio that ball and dehydrated alcohol mass ratio are 1:2:1 is sequentially placed into ball milling in nylon tank and takes out after 4 hours, is put into baker Drying obtains powder at 100~120 DEG C；Powder after drying is added 5wt% polyvinyl alcohol and is granulated, later by pressed by powder It is 12mm with a thickness of the cylinder sample of 6mm at diameter, sample is placed in Muffle furnace and is heated to the heating rate of 1 DEG C/min 550 DEG C and at this temperature dumping 4 hours, the cylinder sample of drained glue is sintered 4 hours at 950~1200 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)

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