CN109650889A - A kind of preparation method of sintering temperature and low dielectric ceramic - Google Patents
A kind of preparation method of sintering temperature and low dielectric ceramic Download PDFInfo
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Abstract
The present invention discloses a kind of preparation method of sintering temperature and low dielectric ceramic, includes the following steps: to take BaO, Nd2O3、TiO2And modifying agent, wet ball-milling mixing 12 hours or more, ball-milling medium was distilled water, is dried after ball milling;Mixed powder after ball milling is sintered 4 hours in 850~880 DEG C of air atmospheres;In powder obtained add binder and be granulated after, re-compacted molding, be finally sintered in 950~990 DEG C of air atmospheres 4 hours to get.Preparation method simple process provided by the invention, it is suitable for large-scale industrialization that sintering temperature is low, sintering time is short, short preparation period, has very vast potential for future development.
Description
Technical field
The present invention relates to technical field of functional ceramics, in particular to a kind of preparation method of sintering temperature and low dielectric ceramic.
Background technique
Microwave-medium ceramics refer to and dielectric material and complete one or more functions applied to being used as in microwave frequency band circuit
Ceramic material.Microwave-medium ceramics as a kind of novel electron material, be used as in modern communications resonator, filter,
Dielectric substrate, diectric antenna, dielectric guided wave circuit etc. are widely used in many fields of microwave technology, such as mobile phone, automobile
Phone, wireless phone, telstar receiver, satellite broadcasting, radar, wireless remotecontrol etc..With LTCC Technology
Continuous development, the application prospects of microwave dielectric ceramic materials can be more preferable.
BLT system microwave ceramics is substantially all the tungsten bronze crystal structure for belonging to perovskite-like.Main phase composition is usually write a Chinese character in simplified form
For Ln (rare earth element)=Pr, Sm, Nd etc., all there is phase within this range for BaOLn2O3nTiO2 (n=3~5)
As crystal structure.BLT system microwave ceramics is widely studied and is applied, which is to have high permittivity εr
>=80, and ε can achieve by addition appropriate modificationrIn 90~100 ranges.Under formula appropriate and process conditions,
Higher Q value and lower TCf value can and be obtained simultaneously.
In addition, existing BLT system microwave ceramics sintering temperature, two methods are generally used in industry, first is that addition eutectic
The glass phase of point, but Qf value reduces obviously;Second method is the powder granule in raw material to be accomplished very small, and granularity is less than
200nm, it is unobvious that this method can guarantee that Qf value reduces, but sintering temperature is still higher than 1350 DEG C, and technical difficulty is big, state
It is interior to cannot achieve at present.
Summary of the invention
In view of the above technical problems, the present invention provides a kind of preparation methods of sintering temperature and low dielectric ceramic, solve existing
The excessively high problem of some BLT system microwave ceramics sintering temperatures.
In order to solve the above technical problems, the technical solution of the present invention is as follows:
The present invention provides a kind of preparation method of sintering temperature and low dielectric ceramic, includes the following steps:
(1) BaO, Nd are taken2O3、TiO2And modifying agent, wet ball-milling mixing 12 hours or more, ball-milling medium was distilled water, ball
It is dried after mill;
(2) mixed powder after ball milling is sintered 4 hours in 850~880 DEG C of air atmospheres;
(3) after adding binder in the powder made from step (2) and being granulated, re-compacted molding, finally 950~990
Be sintered in DEG C air atmosphere 4 hours to get.
Wherein it is preferred to which the modifying agent is CaO, WO that molar ratio is 1:2:13And Fe2O3。
Wherein it is preferred to described BaO, Nd2O3、TiO2Molar ratio with modifying agent is 1:1:X:(0.003~0.015), X
Value is Isosorbide-5-Nitrae or 5.
Wherein it is preferred to which the binder is one of PVA, paraffin and PVB or a variety of.
Wherein it is preferred to which the particle size range for obtaining mixed powder after being granulated in the step (3) is 200 mesh~300 mesh.
Wherein it is preferred to which the weight ratio of powder described in the step (3) and the binder is 100:(15~30).
Beneficial effects of the present invention:
Compared with prior art, microwave-medium ceramics provided by the invention use BaO-Nd2O3-TiO2For basic system, lead to
The modifying agent of overdoping specific components, modifying agent during the sintering process, will form liquid phase, increases sintered density, improve agglutinating property
Can and stability, sintering temperature hereinafter, sintering temperature is low, and realize preferable interaction at 1000 DEG C, improve Jie
Electric constant, but the decline of Q value is unobvious, while temperature coefficient of resonance frequency is adjustable, and sintering temperature is low.The experimental results showed that
The present invention mentions the dielectric constant of microwave-medium ceramics between 90~100, and temperature coefficient of resonance frequency τ f goes to zero and model
It is trapped among adjustable between 70~90ppm/ DEG C, Qf (5GHz) value between 1500~3000, meets novel millimetric wave device
Application requirement.
In addition, preparation method simple process provided by the invention, sintering temperature is low, sintering time is short, short preparation period, fits
Suitable large-scale industrialization, has very vast potential for future development.
Specific embodiment
Below in conjunction with the specific embodiment of the invention, technical solution of the present invention is clearly and completely described, is shown
So, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the reality in the present invention
Example is applied, every other embodiment obtained by those of ordinary skill in the art without making creative efforts all belongs to
In the scope of protection of the invention.
Embodiment 1
The present embodiment provides a kind of preparation methods of sintering temperature and low dielectric ceramic, include the following steps:
(1) BaO, Nd are taken2O3、TiO2And modifying agent, wet ball-milling mix 12 hours, ball-milling medium is distilled water, after ball milling
Drying;The modifying agent is CaO, WO that molar ratio is 1:2:13And Fe2O3;Described BaO, Nd2O3、TiO2With mole of modifying agent
Than for 1:1:4:0.008;
(2) mixed powder after ball milling is sintered 4 hours in 850~880 DEG C of air atmospheres;
(3) after adding PVA in the powder made from step (2) and being granulated, the particle size range of mixed powder is obtained after granulation
For 200 mesh, re-compacted molding, be finally sintered in 950~990 DEG C of air atmospheres 4 hours to get.
Wherein, the weight ratio of powder described in the step (3) and the binder is 100:25.
Ceramics sample to be measured is polished by metallographic, flannelette dielectric surface, using Agilent 5061B Network Analyzer,
Dielectric constant and tan δ are measured according to Hakki-Coleman method, and Qf value is calculated;In addition, temperature coefficient of resonance frequency
Measurement be to be connected directly Network Analyzer and insulating box, test within the temperature range of 20 DEG C~85 DEG C resonance frequency change
Change value, then shown formula calculates τ f value according to the following formula;
The dielectric constant of microwave-medium ceramics manufactured in the present embodiment is 95, and temperature coefficient of resonance frequency τ f is 80ppm/
DEG C, Qf (5GHz) value is 2500.
Embodiment 2
The present embodiment provides a kind of preparation methods of sintering temperature and low dielectric ceramic, include the following steps:
(1) BaO, Nd are taken2O3、TiO2And modifying agent, wet ball-milling mix 15 hours, ball-milling medium is distilled water, after ball milling
Drying;The modifying agent is CaO, WO that molar ratio is 1:2:13And Fe2O3;Described BaO, Nd2O3、TiO2With mole of modifying agent
Than for 1:1:5:0.003~0.015;
(2) mixed powder after ball milling is sintered 4 hours in 850~880 DEG C of air atmospheres;
(3) after adding paraffin in the powder made from step (2) and being granulated, the particle size range of mixed powder is obtained after granulation
For 300 mesh, re-compacted molding, be finally sintered in 950~990 DEG C of air atmospheres 4 hours to get.
Wherein, the weight ratio of powder described in the step (3) and the binder is 100:15~30.
The test method provided according to embodiment 1 is to the properties of microwave-medium ceramics made from the embodiment of the present invention 2
It is tested.
The dielectric constant of microwave-medium ceramics manufactured in the present embodiment is 90, and temperature coefficient of resonance frequency τ f is 85ppm/
Adjustable between DEG C, Qf (5GHz) value is 2000.
Embodiment 3
The present embodiment provides a kind of preparation methods of sintering temperature and low dielectric ceramic, include the following steps:
(1) BaO, Nd are taken2O3、TiO2And modifying agent, wet ball-milling mix 14 hours, ball-milling medium is distilled water, after ball milling
Drying;The modifying agent is CaO, WO that molar ratio is 1:2:13And Fe2O3;Described BaO, Nd2O3、TiO2With mole of modifying agent
Than for 1:1:5:0.015, X value is Isosorbide-5-Nitrae or 5;
(2) mixed powder after ball milling is sintered 4 hours in 850~880 DEG C of air atmospheres;
(3) after adding PVB in the powder made from step (2) and being granulated, the particle size range of mixed powder is obtained after granulation
For 200 mesh, re-compacted molding, be finally sintered in 950~990 DEG C of air atmospheres 4 hours to get.
Wherein, the weight ratio of powder described in the step (3) and the binder is 100:30.
The test method provided according to embodiment 1 is to the properties of microwave-medium ceramics made from the embodiment of the present invention 3
It is tested.
The dielectric constant of microwave-medium ceramics manufactured in the present embodiment is 100, and temperature coefficient of resonance frequency τ f is
70ppm/ DEG C, Qf (5GHz) value is 3000.
Embodiment 4
The present embodiment provides a kind of preparation methods of sintering temperature and low dielectric ceramic, include the following steps:
(1) BaO, Nd are taken2O3、TiO2And modifying agent, wet ball-milling mix 14 hours, ball-milling medium is distilled water, after ball milling
Drying;The modifying agent is CaO, WO that molar ratio is 1:2:13And Fe2O3;Described BaO, Nd2O3、TiO2With mole of modifying agent
Than for 1:1:4:0.010, X value is Isosorbide-5-Nitrae or 5;
(2) mixed powder after ball milling is sintered 4 hours in 850~880 DEG C of air atmospheres;
(3) after adding paraffin in the powder made from step (2) and being granulated, the particle size range of mixed powder is obtained after granulation
For 200 mesh~300 mesh, re-compacted molding, be finally sintered in 950~990 DEG C of air atmospheres 4 hours to get.
Wherein, the weight ratio of powder described in the step (3) and the binder is 100:20.
The test method provided according to embodiment 1 is to the properties of microwave-medium ceramics made from the embodiment of the present invention 4
It is tested.
The dielectric constant of microwave-medium ceramics manufactured in the present embodiment is 92, and temperature coefficient of resonance frequency τ f is 90ppm/
DEG C, Qf (5GHz) value is 2500.
Embodiment 5
The present embodiment provides a kind of preparation methods of sintering temperature and low dielectric ceramic, include the following steps:
(1) BaO, Nd are taken2O3、TiO2And modifying agent, wet ball-milling mix 13 hours, ball-milling medium is distilled water, after ball milling
Drying;The modifying agent is CaO, WO that molar ratio is 1:2:13And Fe2O3;Described BaO, Nd2O3、TiO2With mole of modifying agent
Than for 1:1:1:0.008;
(2) mixed powder after ball milling is sintered 4 hours in 850~880 DEG C of air atmospheres;
(3) after adding PVB in the powder made from step (2) and being granulated, the particle size range of mixed powder is obtained after granulation
For 300 mesh, re-compacted molding, be finally sintered in 950~990 DEG C of air atmospheres 4 hours to get.
Wherein, the weight ratio of powder described in the step (3) and the binder is 100:25.
The test method provided according to embodiment 1 is to the properties of microwave-medium ceramics made from the embodiment of the present invention 5
It is tested.
The dielectric constant of microwave-medium ceramics manufactured in the present embodiment is between 45, and temperature coefficient of resonance frequency τ f is
70ppm/ DEG C, Qf (5GHz) value is 3000.
Comparative example
The present embodiment provides a kind of preparation methods of dielectric ceramic, include the following steps:
(1) BaO, Nd are taken2O3And TiO2, wet ball-milling mixing 12 hours, ball-milling medium is distilled water, is dried after ball milling;Institute
Stating modifying agent is CaO, WO that weight ratio is 1:2:13And Fe2O3;
(2) mixed powder after ball milling is sintered 4 hours in 1350~1380 DEG C of air atmospheres;
(3) after adding PVA in the powder made from step (2) and being granulated, the particle size range of mixed powder is obtained after granulation
For 200 mesh, re-compacted molding, be finally sintered in 1350~1390 DEG C of air atmospheres 4 hours to get.
Wherein, the weight ratio of powder described in the step (3) and the binder is 100:25.
The properties of microwave-medium ceramics made from comparative example are surveyed according to the test method that embodiment 1 provides
Examination.
The dielectric constant of microwave-medium ceramics manufactured in the present embodiment is 65, and temperature coefficient of resonance frequency τ f is 78ppm/
DEG C, Qf (5GHz) value is 2700.
BaO-Nd it can be seen from the microwave-medium ceramics performance made from comparative example2O3-TiO2Dielectric ceramic is to prepare
During, after being not added with modifying agent, sintering temperature is increased, also, compared with the embodiment 1 of addition modifying agent, dielectric constant
It reduces, Qf value increases unobvious.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of preparation method of sintering temperature and low dielectric ceramic, it is characterised in that include the following steps:
(1) BaO, Nd are taken2O3、TiO2And modifying agent, wet ball-milling mix 12 hours or more, ball-milling medium is distilled water, after ball milling
Drying;
(2) mixed powder after ball milling is sintered 4 hours in 850~880 DEG C of air atmospheres;
(3) after adding binder in the powder made from step (2) and being granulated, re-compacted molding is finally big at 950~990 DEG C
Be sintered in gas atmosphere 4 hours to get.
2. a kind of preparation method of sintering temperature and low dielectric ceramic according to claim 1, it is characterised in that: the modification
Agent is CaO, WO that molar ratio is 1:2:13And Fe2O3。
3. a kind of preparation method of sintering temperature and low dielectric ceramic according to claim 2, it is characterised in that: the BaO,
Nd2O3、TiO2Molar ratio with modifying agent is 1:1:X:(0.003~0.015), X value is Isosorbide-5-Nitrae or 5.
4. a kind of preparation method of sintering temperature and low dielectric ceramic according to claim 1, it is characterised in that: the bonding
Agent is one of PVA, paraffin and PVB or a variety of.
5. according to a kind of preparation method for sintering temperature and low dielectric ceramic that claim 4 is stated, it is characterised in that: the step
(3) particle size range that mixed powder is obtained after being granulated in is 200 mesh~300 mesh.
6. according to a kind of preparation method for sintering temperature and low dielectric ceramic that claim 4 is stated, it is characterised in that: the step
(3) weight ratio of powder described in and the binder is 100:(15~30).
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CN113045314A (en) * | 2019-12-27 | 2021-06-29 | 奇力新电子股份有限公司 | Thin ceramic powder suitable for high-frequency assembly |
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Application publication date: 20190419 |