CN107216150A - A kind of low-temperature co-burning ceramic material and preparation method thereof - Google Patents
A kind of low-temperature co-burning ceramic material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of low-temperature co-burning ceramic material and preparation method thereof, the low-temperature co-burning ceramic material is the NaBi of tetragonal crystalline structurexLa(1‑x)(MoO4)2, wherein 0.2≤x≤0.8, average grain diameter is 30 60nm.Low temperature co-fired molybdate composite ceramic material prepared by the present invention has higher dielectric constant (ε r ＞ 10), minimum dielectric loss (Qf ＞ 5000GHz), extremely low temperature coefficient of resonance frequency (TCF ≈ 0ppm/ DEG C) and relatively low sintering temperature (less than common metal Ag, Cu and Al etc. fusing point), do not reacted with Ag etc., it can be used as the base-material of ltcc substrate, encapsulating material, and it is used for a variety of electronic components, such as resonator, wave filter as microwave-medium ceramics.
Description
Technical field
The invention belongs to microwave-medium ceramics technical field, it is related to a kind of low-temperature co-burning ceramic material and preparation method thereof.
Background technology
Microwave-medium ceramics are to be mainly used in microwave frequency band (to be mainly 300MHz~300GHz, corresponding electromagnetic wavelength
For 1m~1mm) in circuit, and the medium ceramic material of one or more functions is played in circuit, it is modern communication electronics member
Device (resonator, oscillator, wave filter, Medium Wave Guide loop, diectric antenna etc.) widely used critical material.With electronics
Circuit develops to miniaturization, integrated and high frequency direction, and it is small, integrated that areas of information technology propose size to electronic component
The requirement that degree is high, cost is low.
It is to burn low temperature using LTCC Technology (Low Temperature Co-fired Ceramic, LTCC)
Thickness accurately fine and close green band is made in knot ceramic powder, and laser boring, micropore slip casting, accurate conductor slurry are utilized on green band
The techniques such as material printing make required circuitous pattern, and by the embedment of multiple passive elements wherein, then overlap together,
Less than 900 DEG C sintering, it is possible to achieve the high integration encapsulation of electronic component, but common microwave-medium ceramics sintering temperature is too high
(fusing point for being higher than common metal), it is impossible to burnt altogether with metal, it is difficult to applied in LTCC Technology, cause microwave-medium
The application of ceramic material is limited by very large.In order to overcome this problem, low temperature co-fired microwave dielectric ceramic powder is developed
Material is necessary.
The content of the invention
The technical problems to be solved by the invention are common there is provided a kind of low temperature for above shortcomings in the prior art
Burn molybdate composite ceramic and preparation method thereof.
In order to solve the above technical problems, the technical scheme that the present invention is provided is：
A kind of low-temperature co-burning ceramic material is provided, the low-temperature co-burning ceramic material is tetragonal crystalline structure
NaBixLa(1-x)(MoO4)2, i.e. bismuth molybdate sodium and lanthanum molybdate sodium lattice substituted type compound, wherein 0.2≤x≤0.8, average grain
Footpath is 30-60nm.
The present invention also provides the preparation method of above-mentioned low-temperature co-burning ceramic material, and it comprises the following steps：
1) five nitric hydrate bismuths and lanthanum nitrate hexahydrate are dissolved in ethanol solution, obtain solution I；
2) sodium molybdate is dissolved in the in the mixed solvent of water and ethanol, polyethylene glycol is then added, solution II is obtained；
3) under vigorous stirring by step 1) resulting solution I and step 2) resulting solution II is mixed, and be uniformly mixing to obtain
Gained mixed liquor, is then transferred in hydrothermal reaction kettle and carries out hydro-thermal reaction, reactor then is naturally cooled into room by mixed liquor
Temperature, product centrifugal filtration and be washed with deionized, dry after obtain low-temperature co-burning ceramic material.
By such scheme, step 1) mol ratio of the five nitric hydrates bismuth and lanthanum nitrate hexahydrate is 0.25-4:1；It is described
Five nitric hydrate bi concns are 0.05-0.5mol/L in solution I.
By such scheme, step 2) volume ratio 1 of the mixed solvent reclaimed water and ethanol:1-2, sodium molybdate and polyethylene glycol
Mass ratio be 1:The concentration of sodium molybdate is 0.2-1mol/L in 0.2-1, solution II.
Preferably, step 2) molecular weight polyethylene glycol be 400-2000.
By such scheme, step 3) the mole sum and molybdenum of five nitric hydrate bismuths and lanthanum nitrate hexahydrate in the mixed liquor
The mol ratio of sour sodium is 1:2.
Preferably, step 3) the mixed liquor reclaimed water volume content be less than 30%.
By such scheme, step 3) hydrothermal reaction condition be 130-180 DEG C at react 1-12h.
Preferably, step 3) hydrothermal reaction kettle in hydrothermal reaction process compactedness be 60-80%.
The beneficial effects of the present invention are：The present invention is using five nitric hydrate bismuths, lanthanum nitrate hexahydrate, sodium molybdate to be main former
Material, lanthanum molybdate bismuth sodium ceramic nano powder is prepared using one-step method, and preparation technology is simple, reaction temperature is gentleer, and products therefrom is
Nanoscale low-temperature co-fired ceramic powder；Low temperature co-fired molybdate composite ceramic material prepared by the present invention has higher dielectric normal
Number (ε r ＞ 10), minimum dielectric loss (Qf ＞ 5000GHz), extremely low temperature coefficient of resonance frequency (TCF ≈ 0ppm/ DEG C) and
Relatively low sintering temperature (less than common metal Ag, Cu and Al etc. fusing point), does not react with Ag etc., can be used as LTCC bases
The base-material of plate, encapsulating material, and it is used for a variety of electronic components, such as resonator, wave filter as microwave-medium ceramics.
Embodiment
To make those skilled in the art more fully understand technical scheme, the present invention is made with reference to embodiment
It is described in further detail.
Unless specific instructions, the reagent used is commercially available chemical reagent or industrial products to following examples.
Embodiment 1
A kind of nanometer lanthanum molybdate bismuth sodium raw powder's production technology, comprises the following steps：
1) by 48.5g (0.1mol) Bi (NO3)3·5H2O,234g(0.4mol)La(NO3)3·6H22L is dissolved under O stirrings
Concentration for 95% ethanol solution in, obtain solution I；
2) by 242g (1mol) Na2MoO4·2H22L ethanol/waters (volume ratio 1 is dissolved under O stirrings:1) in the mixed solvent, it is molten
Xie Hou, is adding 242g polyethylene glycol (PEG molecular weight 2000), is stirring, obtain solution II；
3) under vigorous stirring by step 1) resulting solution I and step 2) resulting solution II mixes, the stirring of gained presoma
After uniform, it is transferred in sealing 5L autoclaves, is warming up to 180 DEG C and reacts 12 hours, reactor is naturally cooled into room temperature,
Products therefrom is dried 2 hours through centrifugal filtration, deionized water washing, gained powder at 150 DEG C, obtains NaBi0.2La0.8(MoO4)2
Nano-powder.
The present embodiment products therefrom is subjected to X-ray diffraction analysis, it was demonstrated that it is single-phase tetragonal crystalline structure；Measure product
Purity is more than 99%, and the average grain diameter of nanocrystal is 60nm, and 650-750 DEG C of sintering temperature, dielectric constant 20~30, dielectric is damaged
15000~20000GHz is consumed, temperature coefficient of resonance frequency is close to zero (TFC<3ppm/℃).
Embodiment 2
A kind of nanometer lanthanum molybdate bismuth sodium raw powder's production technology, comprises the following steps：
1) by 194g (0.4mol) Bi (NO3)3·5H2O and 58.5g (0.1mol) La (NO3)3·6H22L is dissolved under O stirrings
In ethanol solution, solution I is obtained；
2) by 242g (1mol) Na2MoO4·2H22L ethanol/waters (volume ratio 1 is dissolved under O stirrings:1) in the mixed solvent, it is molten
Xie Hou, is adding 48.4g polyethylene glycol (PEG molecular weight 600), is stirring, obtain solution II；
3) under vigorous stirring by step 1) resulting solution I and step 2) resulting solution II mixes, the stirring of gained presoma
After uniform, it is transferred in sealing 5L autoclaves, is warming up to 130 DEG C and reacts 6 hours, reactor is naturally cooled into room temperature,
Products therefrom is dried 12 hours through centrifugal filtration, deionized water washing, gained powder at 800 DEG C, obtains NaBi0.8La0.2
(MoO4)2Nano-powder.
The present embodiment products therefrom is subjected to X-ray diffraction analysis, it was demonstrated that it is single-phase tetragonal crystalline structure, measures product
Purity is more than 99%, the average grain diameter 30nm of nanocrystal, 650-750 DEG C of sintering temperature, dielectric constant 20~30, dielectric loss
15000~20000GHz, temperature coefficient of resonance frequency is close to zero (TFC<3ppm/℃).
Embodiment 3
A kind of nanometer lanthanum molybdate bismuth sodium raw powder's production technology, comprises the following steps：
1) by 48.5g (0.1mol) Bi (NO3)3·5H2O,58.5g(0.1mol)La(NO3)3·6H2It is dissolved under O stirrings
In 500mL95% ethanol solution, solution I is obtained；
2) by 96.8g (0.4mol) Na2MoO4·2H2It is dissolved under O stirrings in 500mL ethanol/water mixed solvents, after dissolving,
50g polyethylene glycol (PEG molecular weight 2000) is being added, is stirring, obtains solution II；
3) under vigorous stirring by step 1) resulting solution I and step 2) resulting solution II mixes, the stirring of gained presoma
After uniform, it is transferred in sealing 5L autoclaves, is warming up to 150 DEG C and reacts 6 hours, reactor is naturally cooled into room temperature,
Products therefrom is dried 6 hours through centrifugal filtration, deionized water washing, gained powder at 100 DEG C, obtains NaBi0.5La0.5(MoO4)2
Nano-powder.
The present embodiment products therefrom is subjected to X-ray diffraction analysis, it was demonstrated that it is single-phase tetragonal crystalline structure, measures product
Purity is more than 99%, the average grain diameter 40nm of nanocrystal, 650-750 DEG C of sintering temperature, dielectric constant 20~30, dielectric loss
15000~20000GHz, temperature coefficient of resonance frequency is close to zero (TFC<3ppm/℃).
Embodiment 4
A kind of nanometer lanthanum molybdate bismuth sodium raw powder's production technology, comprises the following steps：
1) by 97.0g (0.2mol) Bi (NO3)3·5H2O,175.5g(0.3mol)La(NO3)3·6H2It is dissolved under O stirrings
In 2L ethanol solutions, solution I is obtained；
2) by 224.0g (1.0mol) Na2MoO4·2H2It is dissolved under O stirrings in 2L ethanol/water mixed solvents, after dissolving,
100g polyethylene glycol (PEG molecular weight 400) is added, stirs, obtains solution II；
3) under vigorous stirring by step 1) resulting solution I and step 2) resulting solution II mixes, the stirring of gained presoma
After uniform, it is transferred in sealing 5L autoclaves, is warming up to 180 DEG C and reacts 1 hour, reactor is naturally cooled into room temperature,
Products therefrom is dried 6 hours through centrifugal filtration, deionized water washing, gained powder at 100 DEG C, obtains NaBi0.4La0.6(MoO4)2
Nano-powder.
The present embodiment products therefrom is subjected to X-ray diffraction analysis, it was demonstrated that it is single-phase tetragonal crystalline structure, measures product
Purity is more than 99%, the average grain diameter 35nm of nanocrystal, 650-750 DEG C of sintering temperature, dielectric constant 20~30, dielectric loss
15000~20000GHz, temperature coefficient of resonance frequency is close to zero (TFC<3ppm℃).
Claims (6)
1. a kind of low-temperature co-burning ceramic material, it is characterised in that the low-temperature co-burning ceramic material is tetragonal crystalline structure
NaBixLa(1-x)(MoO4)2, wherein 0.2≤x≤0.8, average grain diameter is 30-60nm.
2. the preparation method of the low-temperature co-burning ceramic material described in a kind of claim 1, it is characterised in that comprise the following steps：
1) five nitric hydrate bismuths and lanthanum nitrate hexahydrate are dissolved in ethanol solution, obtain solution I；
2) sodium molybdate is dissolved in the in the mixed solvent of water and ethanol, polyethylene glycol is then added, solution II is obtained；
3) under vigorous stirring by step 1) resulting solution I and step 2) resulting solution II is mixed, and it is uniformly mixing to obtain mixing
Gained mixed liquor, is then transferred in hydrothermal reaction kettle and carries out hydro-thermal reaction, reactor then is naturally cooled into room temperature by liquid, production
Thing centrifugal filtration and be washed with deionized, dry after obtain low-temperature co-burning ceramic material.
3. preparation method according to claim 2, it is characterised in that step 1) the five nitric hydrates bismuth and six water nitric acid
The mol ratio of lanthanum is 0.25-4:1；Five nitric hydrate bi concns are 0.05-0.5mol/L in the solution I.
4. preparation method according to claim 2, it is characterised in that step 2) body of the mixed solvent reclaimed water and ethanol
Product compares 1:The mass ratio of 1-2, sodium molybdate and polyethylene glycol is 1:The concentration of sodium molybdate is 0.2-1mol/L in 0.2-1, solution II.
5. preparation method according to claim 2, it is characterised in that step 3) in the mixed liquor five nitric hydrate bismuths with
The mole sum of lanthanum nitrate hexahydrate and the mol ratio of sodium molybdate are 1:2.
6. preparation method according to claim 2, it is characterised in that step 3) hydrothermal reaction condition is 130-180 DEG C
Lower reaction 1-12h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110668817A (en) * | 2019-10-31 | 2020-01-10 | 西安交通大学 | Sodium-based composite microwave dielectric ceramic material sintered at ultralow temperature and preparation method thereof |
| CN113087525A (en) * | 2021-03-31 | 2021-07-09 | 中国振华集团云科电子有限公司 | Molybdate-based composite microwave dielectric ceramic material and preparation method thereof |
| CN115947600A (en) * | 2022-10-11 | 2023-04-11 | 电子科技大学 | Li-Mg-Mo-based single-phase ultralow-temperature ceramic material and preparation method thereof |
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| CN110668817A (en) * | 2019-10-31 | 2020-01-10 | 西安交通大学 | Sodium-based composite microwave dielectric ceramic material sintered at ultralow temperature and preparation method thereof |
| CN113087525A (en) * | 2021-03-31 | 2021-07-09 | 中国振华集团云科电子有限公司 | Molybdate-based composite microwave dielectric ceramic material and preparation method thereof |
| CN113087525B (en) * | 2021-03-31 | 2023-04-18 | 中国振华集团云科电子有限公司 | Molybdate-based composite microwave dielectric ceramic material and preparation method thereof |
| CN115947600A (en) * | 2022-10-11 | 2023-04-11 | 电子科技大学 | Li-Mg-Mo-based single-phase ultralow-temperature ceramic material and preparation method thereof |
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