CN108947530A - A kind of low transparent Re of dielectric of garnet structurexGd3-xAl3Ga2O12Microwave ceramics and preparation method thereof - Google Patents

A kind of low transparent Re of dielectric of garnet structurexGd3-xAl3Ga2O12Microwave ceramics and preparation method thereof Download PDF

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CN108947530A
CN108947530A CN201810908551.6A CN201810908551A CN108947530A CN 108947530 A CN108947530 A CN 108947530A CN 201810908551 A CN201810908551 A CN 201810908551A CN 108947530 A CN108947530 A CN 108947530A
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transparent
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袁昌来
蒙柳方
廖燕君
刘笑
朱保华
刘飞
许积文
周昌荣
陈国华
饶光辉
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Guilin University of Electronic Technology
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Abstract

The invention discloses a kind of transparent Re of the low dielectric of garnet structurexGd3‑xAl3Ga2O12Microwave ceramics and preparation method thereof, it is Re which, which forms general formula,xGd3‑xAl3Ga2O12, wherein 0≤x≤ 0.065, Re are one of Nd and Er.Conventional solid synthetic method is first used to synthesize Re when preparationxGd3‑xAl3Ga2O12Powder, then the powder of synthesis and 5% PVAC polyvinylalcohol are mixed and dried according to the ratio of 0.5mL:10g, grind into powder；Powder is finally pressed into ceramic body, 15 ~ 60 hours is kept the temperature at 1580 ~ 1650 DEG C and is made.The low transparent microwave ceramics of dielectric of garnet structure prepared by the present invention, dielectric constant (ε r ) between 9.7 ~ 10.3, quality factor and resonance frequency product (Q.f) between 1600 ~ 5100GHz, temperature coefficient of resonance frequency (T cf ) between -25 ~ -80ppm/ DEG C, show that the present invention successfully prepares a kind of low transparent microwave ceramics of dielectric of garnet structure.This microwave ceramics can be used for manufacturing microwave-medium component such as filter, resonator, medium substrate etc., in particular in the information communication and integrated circuit of visualization transparent window.

Description

A kind of low transparent Re of dielectric of garnet structurexGd3-xAl3Ga2O12Microwave ceramics and its system Preparation Method
Technical field
The invention belongs to informational function microwave ceramics manufacturing fields, and in particular to a kind of low dielectric of garnet structure is transparent RexGd3-xAl3Ga2O12Microwave ceramics and preparation method thereof.
Background technique
With the rapid development of modern communication and Radar Technology, microwave communication has constituted the important composition of modern communications technology Part.Compared with common radio wave, microwave is high with frequency, wavelength is short, strong antijamming capability, can penetrate the spies such as ionosphere Point, suitable for making large capacity, high quality, the signal vehicle of telecommunication.Dielectric constant (ε r ), dielectric loss (tanδ) and resonance Frequency-temperature coefficient (τ f ) it is the major parameter for evaluating microwave-medium ceramics dielectric properties.The transmitance of microwave-medium ceramics be compared with The direction of few researcher's concern.
Currently, improving there are mainly two types of the methods of ceramic material transmitance: another then be one is ionic compartmentation is modified Improve sintering technology.
It is consulted, has been reported that discovery spinel-type MgAl2O4Ceramics are also shown while with microwave dielectric property Bright feature；And the Re of garnet structure3Ga5O12(Re:Nd, Sm, Eu, Dy, Yb, Y) and Re3Al5O12(RE:Tb, Y, Er, Yb) Ceramics all have excellent microwave dielectric property, but it is opaque ceramic material.Inventor is it was found that, garnet knot The Al-Ga system of structure can have certain transparent feature when with microwave dielectric property simultaneously.Based on this, inventor to its into Row ionic compartmentation is modified, and extends the sintered heat insulating time, prepares a kind of low transparent microwave ceramics of dielectric of garnet structure.
Summary of the invention
The purpose of the present invention is to provide a kind of transparent Re of the low dielectric of garnet structurexGd3-xAl3Ga2O12Microwave ceramics and Preparation method.
The low transparent Re of dielectric of garnet structure of the present inventionxGd3-xAl3Ga2O12Microwave ceramics forms general formula are as follows: RexGd3-xAl3Ga2O12, wherein 0≤x≤ 0.065, Re are one of Nd and Er.
The low transparent Re of dielectric of garnet structure of the present inventionxGd3-xAl3Ga2O12The preparation method of microwave ceramics, including Following steps:
(1) Re is synthesized using conventional solid synthetic methodxGd3-xAl3Ga2O12Powder；
Select purity for 99.9%Re2O3、99.9%Gd2O3、99.5%Al2O3、99.9%Ga2O3Powder is raw material, according to Re2O3: Gd2O3:Al2O3:Ga2O3= x:3-x: the molar ratio mixing of 3:2, wherein 0≤x≤0.065；
Using dehydrated alcohol as medium, take dehydrated alcohol and mixed powder according to 10mL(dehydrated alcohol): 10g(mixed powder End) ratio mixing after, be placed in planetary ball mill and be sufficiently mixed for 24 hours, take out drying, grinding is 5 small using 1100 DEG C of heat preservations Shi Hecheng RexGd3-xAl3Ga2O12Powder；
(2) Re synthesized using step (1)xGd3-xAl3Ga2O12Powder and 5% polyvinyl alcohol (PVA) are according to 10g: 0.5mL Ratio be mixed and dried, grind into powder；
(3) powder of step (2) is pressed into ceramic body, keeps the temperature 15 ~ 60 hours at 1580 ~ 1650 DEG C to get garnet is arrived The transparent Re of the low dielectric of structurexGd3-xAl3Ga2O12Microwave ceramics.
Under normal conditions, improve ceramic microwave dielectric properties or transparency, the ceramics of various structures need to take using ion In generation, is modified.Inventor is by a large amount of experiment, in garnet structure Gd3Ga5O12In system, the element al of the same valence state of Ga, The part such as Cr, Bi replaces, and only Al replaces (chemical formula Gd3Al3Ga2O12) it can be realized certain transparency, further saturating Bright Gd3Al3Ga2O12Replacing Gd with part Nd or Er in system, ceramics still show transparent feature, and other rare earth element y b, The substitutions such as Sm, Dy are then no longer transparent.Therefore, Gd of the present invention to garnet structure3Ga5O12Ceramics carry out ionic compartmentation and are modified, Use Al3+Part replaces Ga3+, Nd or the part Er replace Gd3+, using conventional solid sintering process, extend the sintered heat insulating time, preparation RexGd3-xAl3Ga2O12Ceramics successfully realize the ceramics transparency, test through microwave dielectric property, ceramic microwave dielectric constant (ε r ) between 9.7 ~ 10.3, quality factor and resonance frequency product (Q.f) between 1600 ~ 5100GHz, temperature coefficient of resonance frequency (T cf ) between -25 ~ -80ppm/ DEG C, this shows that the present invention successfully prepares a kind of low transparent microwave ceramics of dielectric of garnet structure. This microwave ceramics can be used for manufacturing microwave-medium component such as filter, resonator, medium substrate etc., in particular for visual In the information communication and integrated circuit for changing transparent window.
Detailed description of the invention
Fig. 1 is 1 Gd of embodiment3Al3Ga2O12Sintering temperature soaking time at 1625 DEG C is respectively 15,30,45,60 small When sample.
Fig. 2 is 2 Nd of embodiment0.008Gd2.992Al3Ga2O12Sintering temperature soaking time at 1625 DEG C is respectively 15, 30,45,60 hours samples.
Fig. 3 is 3 Nd of embodiment0.018Gd2.982Al3Ga2O12Sintering temperature soaking time at 1625 DEG C is respectively 15, 30,45,60 hours samples.
Fig. 4 is 4 Nd of embodiment0.045Gd2.955Al3Ga2O12Sintering temperature soaking time at 1625 DEG C is respectively 15, 30,45,60 hours samples.
Fig. 5 is 5 Nd of embodiment0.065Gd2.935Al3Ga2O12Sintering temperature soaking time at 1625 DEG C is respectively 15, 30,45,60 hours samples.
Fig. 6 is 6 Er of embodiment0.008Gd2.992Al3Ga2O12Sintering temperature soaking time at 1625 DEG C is respectively 15, 30,45,60 hours samples.
Fig. 7 is 7 Er of embodiment0.018Gd2.982Al3Ga2O12Sintering temperature soaking time at 1625 DEG C is respectively 15, 30,45,60 hours samples.
Fig. 8 is 8 Er of embodiment0.045Gd2.955Al3Ga2O12Sintering temperature soaking time at 1625 DEG C is respectively 15, 30,45,60 hours samples.
Fig. 9 is 9 Er of embodiment0.065Gd2.935Al3Ga2O12Sintering temperature soaking time at 1625 DEG C is respectively 15, 30,45,60 hours samples.
Specific embodiment
The content of present invention is further described below with reference to nine embodiments, but is not limitation of the invention.
Embodiment 1:
Prepare the transparent Gd of the low dielectric of garnet structure3Al3Ga2O12Microwave ceramics includes the following steps:
(1) Gd of high-purity is selected2O3(99.9%), Al2O3(99.5%), Ga2O3(99.9%) powder is raw material, by Gd2O3 : Al2O3: Ga2O3The molar ratio of=3:3:2 mixes；
Using dehydrated alcohol as medium, take dehydrated alcohol and mixed powder according to 10mL(dehydrated alcohol): 10g(mixed powder End) ratio mixing after, be placed in planetary ball mill and be sufficiently mixed for 24 hours, take out drying, grinding is 5 small using 1100 DEG C of heat preservations Shi Hecheng Gd3Al3Ga2O12Powder；
(2) gained powder and 5% PVA are mixed and dried according to 10g: 0.5mL ratio, grind into powder；
(3) powder is pressed into ceramic body, keeps the temperature 15 ~ 60 hours at 1580 ~ 1650 DEG C to get the low dielectric of garnet structure is arrived Transparent Gd3Al3Ga2O12Microwave ceramics.
The Gd of preparation3Al3Ga2O12Test result is as follows through microwave dielectric property for microwave ceramics:
Gd3Al3Ga2O12Sintering temperature soaking time at 1625 DEG C is respectively 15,30,45,60 hours sample such as Fig. 1 institutes Show, sample has certain transparent feature.
Embodiment 2:
Prepare the transparent Nd of the low dielectric of garnet structure0.008Gd2.992Al3Ga2O12Microwave ceramics includes the following steps:
(1) Nd of high-purity is selected2O3(99.9%), Gd2O3(99.9%), Al2O3(99.5%), Ga2O3(99.9%) powder is original Material, according to Nd2O3: Gd2O3: Al2O3: Ga2O3The molar ratio of=0.008:2.992:3:2 mixes；
Using dehydrated alcohol as medium, take dehydrated alcohol and mixed powder according to 10mL(dehydrated alcohol): 10g(mixed powder End) ratio mixing after, be placed in planetary ball mill and be sufficiently mixed for 24 hours, take out drying, grinding is 5 small using 1100 DEG C of heat preservations Shi Hecheng Nd0.008Gd2.992Al3Ga2O12Powder；
(2) gained powder and 5% PVA are mixed and dried according to 10g: 0.5mL ratio, grind into powder；(3) by powder It is pressed into ceramic body, keeps the temperature 15 ~ 60 hours at 1580 ~ 1650 DEG C to get transparent to the low dielectric of garnet structure Nd0.008Gd2.992Al3Ga2O12Microwave ceramics.
The Nd of preparation0.008Gd2.992Al3Ga2O12Test result is as follows through microwave dielectric property for microwave ceramics:
Nd0.008Gd2.992Al3Ga2O12Sintering temperature soaking time at 1625 DEG C is respectively 15,30,45,60 hours samples As shown in Fig. 2, sample has certain transparent feature.
Embodiment 3:
Prepare the transparent Nd of the low dielectric of garnet structure0.018Gd2.982Al3Ga2O12Microwave ceramics includes the following steps:
(1) Nd of high-purity is selected2O3(99.9%), Gd2O3(99.9%), Al2O3(99.5%), Ga2O3(99.9%) powder is original Material, according to Nd2O3: Gd2O3: Al2O3: Ga2O3The molar ratio of=0.018:2.982:3:2 mixes；
Using dehydrated alcohol as medium, take dehydrated alcohol and mixed powder according to 10mL(dehydrated alcohol): 10g(mixed powder End) ratio mixing after, be placed in planetary ball mill and be sufficiently mixed for 24 hours, take out drying, grinding is 5 small using 1100 DEG C of heat preservations Shi Hecheng Nd0.018Gd2.982Al3Ga2O12Powder；
(2) gained powder and 5% PVA are mixed and dried according to 10g: 0.5mL ratio, grind into powder；
(3) powder is pressed into ceramic body, keeps the temperature 15 ~ 60 hours at 1580 ~ 1650 DEG C to get the low dielectric of garnet structure is arrived Transparent Nd0.018Gd2.982Al3Ga2O12Microwave ceramics.
The Nd of preparation0.018Gd2.982Al3Ga2O12Test result is as follows through microwave dielectric property for microwave ceramics:
Nd0.018Gd2.982Al3Ga2O12Sintering temperature soaking time at 1625 DEG C is respectively 15,30,45,60 hours samples As shown in figure 3, sample has certain transparent feature.
Embodiment 4:
Prepare the transparent Nd of the low dielectric of garnet structure0.045Gd2.955Al3Ga2O12Microwave ceramics includes the following steps:
(1) Nd of high-purity is selected2O3(99.9%), Gd2O3(99.9%), Al2O3(99.5%), Ga2O3(99.9%) powder is original Material, according to Nd2O3: Gd2O3: Al2O3: Ga2O3The molar ratio of=0.045:2.955:3:2 mixes；
Using dehydrated alcohol as medium, take dehydrated alcohol and mixed powder according to 10mL(dehydrated alcohol): 10g(mixed powder End) ratio mixing after, be placed in planetary ball mill and be sufficiently mixed for 24 hours, take out drying, grinding is 5 small using 1100 DEG C of heat preservations Shi Hecheng Nd0.045Gd2.955Al3Ga2O12Powder；
(2) gained powder and 5% PVA are mixed and dried according to 10g: 0.5mL ratio, grind into powder；
(3) powder is pressed into ceramic body, keeps the temperature 15 ~ 60 hours at 1580 ~ 1650 DEG C to get the low dielectric of garnet structure is arrived Transparent Nd0.045Gd2.955Al3Ga2O12Microwave ceramics.
The Nd of preparation0.045Gd2.955Al3Ga2O12Test result is as follows through microwave dielectric property for microwave ceramics:
Nd0.045Gd2.955Al3Ga2O12Sintering temperature soaking time at 1625 DEG C is respectively 15,30,45,60 hours samples As shown in figure 4, sample has certain transparent feature.
Embodiment 5:
Prepare the transparent Nd of the low dielectric of garnet structure0.065Gd2.935Al3Ga2O12Microwave ceramics includes the following steps:
(1) Nd of high-purity is selected2O3(99.9%), Gd2O3(99.9%), Al2O3(99.5%), Ga2O3(99.9%) powder is original Material, according to Nd2O3: Gd2O3: Al2O3: Ga2O3The molar ratio of=0.065:2.935:3:2 mixes；
Using dehydrated alcohol as medium, take dehydrated alcohol and mixed powder according to 10mL(dehydrated alcohol): 10g(mixed powder End) ratio mixing after, be placed in planetary ball mill and be sufficiently mixed for 24 hours, take out drying, grinding is 5 small using 1100 DEG C of heat preservations Shi Hecheng Nd0.065Gd2.935Al3Ga2O12Powder；
(2) gained powder and 5% PVA are mixed and dried according to 10g: 0.5mL ratio, grind into powder；
(3) powder is pressed into ceramic body, keeps the temperature 15 ~ 60 hours at 1580 ~ 1650 DEG C to get the low dielectric of garnet structure is arrived Transparent Nd0.065Gd2.935Al3Ga2O12Microwave ceramics.
The Nd of preparation0.065Gd2.935Al3Ga2O12Test result is as follows through microwave dielectric property for microwave ceramics:
Nd0.065Gd2.935Al3Ga2O12Sintering temperature soaking time at 1625 DEG C is respectively 15,30,45,60 hours samples As shown in figure 5, sample has certain transparent feature.
Embodiment 6:
Prepare the transparent Er of the low dielectric of garnet structure0.008Gd2.992Al3Ga2O12Microwave ceramics includes the following steps:
(1) Er of high-purity is selected2O3(99.9%), Gd2O3(99.9%), Al2O3(99.5%), Ga2O3(99.9%) powder is original Material, according to Er2O3: Gd2O3: Al2O3: Ga2O3The molar ratio of=0.008:2.992:3:2 mixes；
Using dehydrated alcohol as medium, take dehydrated alcohol and mixed powder according to 10mL(dehydrated alcohol): 10g(mixed powder End) ratio mixing after, be placed in planetary ball mill and be sufficiently mixed for 24 hours, take out drying, grinding is 5 small using 1100 DEG C of heat preservations Shi Hecheng Er0.008Gd2.992Al3Ga2O12Powder；
(2) gained powder and 5% PVA are mixed and dried according to 10g: 0.5mL ratio, grind into powder；
(3) powder is pressed into ceramic body, keeps the temperature 15 ~ 60 hours at 1580 ~ 1650 DEG C to get the low dielectric of garnet structure is arrived Transparent Er0.008Gd2.992Al3Ga2O12Microwave ceramics.
The Er of preparation0.008Gd2.992Al3Ga2O12Test result is as follows through microwave dielectric property for microwave ceramics:
Er0.008Gd2.992Al3Ga2O12Sintering temperature soaking time at 1625 DEG C is respectively 15,30,45,60 hours samples As shown in fig. 6, sample has certain transparent feature.
Embodiment 7:
Prepare the transparent Er of the low dielectric of garnet structure0.018Gd2.982Al3Ga2O12Microwave ceramics includes the following steps:
(1) Er of high-purity is selected2O3(99.9%), Gd2O3(99.9%), Al2O3(99.5%), Ga2O3(99.9%) powder is original Material, according to Er2O3: Gd2O3: Al2O3: Ga2O3The molar ratio of=0.018:2.982:3:2 mixes；
Using dehydrated alcohol as medium, take dehydrated alcohol and mixed powder according to 10mL(dehydrated alcohol): 10g(mixed powder End) ratio mixing after, be placed in planetary ball mill and be sufficiently mixed for 24 hours, take out drying, grinding is 5 small using 1100 DEG C of heat preservations Shi Hecheng Er0.018Gd2.982Al3Ga2O12Powder；
(2) gained powder and 5% PVA are mixed and dried according to 10g: 0.5mL ratio, grind into powder；
(3) powder is pressed into ceramic body, keeps the temperature 15 ~ 60 hours at 1580 ~ 1650 DEG C to get the low dielectric of garnet structure is arrived Transparent Er0.018Gd2.982Al3Ga2O12Microwave ceramics.
The Er of preparation0.018Gd2.982Al3Ga2O12Test result is as follows through microwave dielectric property for microwave ceramics:
Er0.018Gd2.982Al3Ga2O12Sintering temperature soaking time at 1625 DEG C is respectively 15,30,45,60 hours samples As shown in fig. 7, sample has certain transparent feature.
Embodiment 8:
Prepare the transparent Er of the low dielectric of garnet structure0.045Gd2.955Al3Ga2O12Microwave ceramics includes the following steps:
(1) Er of high-purity is selected2O3(99.9%), Gd2O3(99.9%), Al2O3(99.5%), Ga2O3(99.9%) powder is original Material, according to Er2O3: Gd2O3: Al2O3: Ga2O3The molar ratio of=0.045:2.955:3:2 mixes；
Using dehydrated alcohol as medium, take dehydrated alcohol and mixed powder according to 10mL(dehydrated alcohol): 10g(mixed powder End) ratio mixing after, be placed in planetary ball mill and be sufficiently mixed for 24 hours, take out drying, grinding is 5 small using 1100 DEG C of heat preservations Shi Hecheng Er0.045Gd2.955Al3Ga2O12Powder；
(2) gained powder and 5% PVA are mixed and dried according to 10g: 0.5mL ratio, grind into powder；(3) by powder It is pressed into ceramic body, keeps the temperature 15 ~ 60 hours at 1580 ~ 1650 DEG C to get transparent to the low dielectric of garnet structure Er0.045Gd2.955Al3Ga2O12Microwave ceramics.
The Er of preparation0.045Gd2.955Al3Ga2O12Test result is as follows through microwave dielectric property for microwave ceramics:
Er0.045Gd2.955Al3Ga2O12Sintering temperature soaking time at 1625 DEG C is respectively 15,30,45,60 hours samples Product are as shown in figure 8, sample has certain transparent feature.
Embodiment 9:
Prepare the transparent Er of the low dielectric of garnet structure0.065Gd2.935Al3Ga2O12Microwave ceramics includes the following steps:
(1) Er of high-purity is selected2O3(99.9%), Gd2O3(99.9%), Al2O3(99.5%), Ga2O3(99.9%) powder is original Material, according to Er2O3: Gd2O3: Al2O3: Ga2O3The molar ratio of=0.065:2.935:3:2 mixes；
Using dehydrated alcohol as medium, take dehydrated alcohol and mixed powder according to 10mL(dehydrated alcohol): 10g(mixed powder End) ratio mixing after, be placed in planetary ball mill and be sufficiently mixed for 24 hours, take out drying, grinding is 5 small using 1100 DEG C of heat preservations Shi Hecheng Er0.065Gd2.935Al3Ga2O12Powder；
(2) gained powder and 5% PVA are mixed and dried according to 10g: 0.5mL ratio, grind into powder；
(3) powder is pressed into ceramic body, keeps the temperature 15 ~ 60 hours at 1580 ~ 1650 DEG C to get the low dielectric of garnet structure is arrived Transparent Er0.065Gd2.935Al3Ga2O12Microwave ceramics.
The Er of preparation0.065Gd2.935Al3Ga2O12Test result is as follows through microwave dielectric property for microwave ceramics:
Er0.065Gd2.935Al3Ga2O12Sintering temperature soaking time at 1625 DEG C is respectively 15,30,45,60 hours samples As shown in figure 9, sample has certain transparent feature.

Claims (2)

1. a kind of low transparent Re of dielectric of garnet structurexGd3-xAl3Ga2O12Microwave ceramics, it is characterized in that: the microwave ceramics forms General formula is RexGd3-xAl3Ga2O12, wherein 0≤x≤ 0.065, Re are one of Nd and Er.
2. a kind of low transparent Re of dielectric of garnet structure described in claim 1xGd3-xAl3Ga2O12The preparation side of microwave ceramics Method, it is characterized in that: including the following steps:
(1) Re is synthesized using conventional solid synthetic methodxGd3-xAl3Ga2O12Powder；
Select purity for 99.9%Re2O3、99.9%Gd2O3、99.5%Al2O3、99.9%Ga2O3Powder is raw material, according to Re2O3: Gd2O3:Al2O3:Ga2O3= x:3-x: the molar ratio mixing of 3:2, wherein 0≤x≤0.065；
Using dehydrated alcohol as medium, after taking dehydrated alcohol and mixed powder to mix according to the ratio of 10mL:10g, it is placed in row It is sufficiently mixed in celestial body grinding machine for 24 hours, takes out drying, grinding, using 1100 DEG C of heat preservations, 5 hours synthesis RexGd3-xAl3Ga2O12Powder Body；
(2) Re synthesized using step (1)xGd3-xAl3Ga2O12Powder and 5% polyvinyl alcohol according to 10g: 0.5mL ratio It is mixed and dried, grind into powder；
(3) powder of step (2) is pressed into ceramic body, keeps the temperature 15 ~ 60 hours at 1580 ~ 1650 DEG C to get garnet is arrived The transparent Re of the low dielectric of structurexGd3-xAl3Ga2O12Microwave ceramics.
CN201810908551.6A 2018-08-10 2018-08-10 A kind of low transparent Re of dielectric of garnet structurexGd3-xAl3Ga2O12Microwave ceramics and preparation method thereof Withdrawn CN108947530A (en)

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Application publication date: 20181207