CN104310992A - Molten-salt-method synthesized La2O3-MgO-TiO2 dielectric ceramic sintering powder and sintering method thereof - Google Patents
Molten-salt-method synthesized La2O3-MgO-TiO2 dielectric ceramic sintering powder and sintering method thereof Download PDFInfo
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Abstract
The invention relates to a molten-salt-method synthesized dielectric ceramic powder technology and in particular relates to molten-salt-method synthesized La2O3-MgO-TiO2 dielectric ceramic sintering powder and a sintering method thereof. The sintering method comprises the following steps: (1) preparing proportions of raw materials; (2) pre-synthesizing (main parameters: the temperature is 750-850 DEG C and the synthesizing time is 2-4h); (3) finally synthesizing (main parameters: the temperature is 950-1050 DEG C and the synthesizing time is 1-2h); and (4) separating and collecting products. The preparation raw materials are low in cost, the process is short, devices are simple, solid, liquid and gas wastes are not discharged, secondary pollution can not be caused, and MgO, La2O3 and TiO2 oxide powder can be directly synthesized to MgO-La2O3-TiO2 dielectric ceramic sintering powder with low cost.
Description
Technical field
The present invention relates to molten-salt growth method synthesis dielectric ceramic powder technology, specifically a kind of molten-salt growth method synthesis La
2o
3-MgO-TiO
2be dielectric ceramic sintering powder and sintering method thereof.
Background technology
At present, La is similar to
2o
3-MgO-TiO
2the production process of the composite oxides class modern functions Modern Ceramic Material and products thereof of system generally comprises the unit operation such as Feedstock treating and processing, batching and abrasive material batch mixing, shaping, sintering, product performance detection.Normally will pass through the powder raw materials such as the many oxide of processing by necessarily preparing burden, therefore, the quality of the powder raw material needed in plant produced composite oxides is then most important.Current, the powder fineness adopting mechanical processing method (as ball milling, vibration mill and comminution by gas stream etc.) to prepare in industrial production is limited.And superfine-material often adopts chemical process to prepare, can make that material particular diameter is little, even, good fluidity, active large, formability and coking property be better.Open up that one has that synthesis temperature is low, the reaction times is short, product purity that is easy and simple to handle, synthesis is high, the feature such as the crystal formation of powder granule and morphology controllable, the preparation new way meeting the requirement of modern times " green " metallurgical technology then has practical significance.
Molten-salt synthesis is a kind of inorganic materials synthetic method that RECENT DEVELOPMENTS is got up, and compares with other synthetic method, and operating process is simple, does not need other specific equipment.Main process is at high temperature dissolved in the melt of low melting point by oxide crystal, then by slow cooling or other method, forms supersaturated solution, and oxide crystal is reset by being diffused in fused salt, forming core thus new oxide crystal is separated out mutually.First BaFe has been synthesized by molten-salt growth method from Arendt in 1973
12o
19and SrFe
12o
19since, the method obtains and studies widely in synthesizing ceramic powder.In recent years, along with deepening continuously of research, the advantage of molten-salt synthesis shows gradually, and range of application is also more and more extensive, has prepared many oxide powder, as: ZnTiO
3, CaBi
2nb
2o
9deng.
Summary of the invention
The present invention seeks to for existing La
2o
3-MgO-TiO
2be the weak point of humiceram precursor powder (sintering powder), provide a kind of by La
2o
3, MgO, TiO
2oxide compound direct molten-salt growth method synthesis La
2o
3-MgO-TiO
2be dielectric ceramic sintering powder and sintering method thereof.
Technical solution of the present invention: a kind of molten-salt growth method synthesis La
2o
3-MgO-TiO
2be dielectric ceramic sintering powder, by KCl, NaCl, CaCl not containing crystal water
2in any two kinds of villaumites and not containing the granularity 100-200 object La of crystal water
2o
3, MgO, TiO
2oxide powder sintering forms; MgO, TiO
2it is 30 ~ 50% that mixture accounts for pre-synthesis reaction system material molar content, wherein MgO:TiO
2mol ratio is 1:1; KCl, NaCl, CaCl
2in any two kinds of villaumite mixtures to account for pre-synthesis reaction system material molar content be 50 ~ 70%, villaumite mixing mol ratio is 1:1; La
2o
3account for La
2o
3, MgO, TiO
2the molar content of material total amount is 1 ~ 2%.
A kind of molten-salt growth method synthesis La
2o
3-MgO-TiO
2be dielectric ceramic sintering powder sintering method: comprise the following steps:
(1) proportioning starting material:
By KCl, NaCl, CaCl not containing crystal water
2in any two kinds of villaumites be the medium of building-up reactions, not containing the granularity 100-200 object La of crystal water
2o
3, MgO, TiO
2oxide powder is primitive reaction material;
Ratio requirement:
Pre-synthesis system: MgO, TiO
2it is 30 ~ 50% that mixture accounts for pre-synthesis reaction system material molar content, wherein MgO:TiO
2mol ratio is 1:1; KCl, NaCl, CaCl
2in any two kinds of villaumite mixtures to account for pre-synthesis reaction system material molar content be 50 ~ 70%, villaumite mixing mol ratio is 1:1;
Whole synthetic system: La
2o
3account for La
2o
3, MgO, TiO
2the molar content 1 ~ 2% of material total amount adds pre-synthesis system;
(2) pre-synthesis:
Abundant dewatered raw material, with MgO, TiO of above-mentioned steps (1) described content
2kCl, NaCl, CaCl of mixed oxide and mol ratio 1:1
2in villaumite, any two kinds of mixing salts fully mix, and load reactor, require to react 2-4h at temperature 750 ~ 850 DEG C;
(3) synthesis eventually:
System to pre-synthesis adds the La of above-mentioned steps (1) described content
2o
3, at temperature 950 ~ 1050 DEG C reaction 1-2h;
(4) collection of product:
After distilled water cleaning reaction thing, its insoluble solid particle drying and obtain end product-La
2o
3-MgO-TiO
2it is dielectric ceramic sintering powder.
Not containing KCl, NaCl, CaCl of crystal water
2villaumite is by KCl, NaCl, the CaCl containing crystal water
2the villaumite 48h that dewaters at 300 DEG C of temperature in atmosphere obtains.
Not containing the granularity 100-200 object La of crystal water
2o
3, MgO, TiO
2oxide powder is by granularity 100-200 object La
2o
3, MgO, TiO
2oxide powder in atmosphere at 150 DEG C of temperature dry 24h obtain.
Major control condition and foundation:
1, Reactive Synthesis temperature will make the substance system of set proportioning fully melt and reach suitable activity, and the volatile quantity of fused salt is 3-5%, and OK range is 750 ~ 1050 DEG C.
2, the Reactive Synthesis time is wanted fully, and OK range is 1 ~ 4h.
The present invention use raw materials cost and existing technics comparing low by 20%, technical process shorten nearly 30%, equipment simple, can with lower cost directly by La
2o
3, MgO, TiO
2oxide powder prepares La
2o
3-MgO-TiO
2be dielectric ceramic precursor powder, product particle size is little and even, and economical efficiency significantly improves.
Embodiment
Dielectric ceramic is mainly used in making ceramic condenser and microwave-medium element, at MgTiO
3dielectric ceramic adds La rare earth element can significantly improve its dielectric properties.The useful La of admixture
2o
3modification is carried out to thermally-stabilised electrical condenser magnesium titanate ceramics, the La obtained
2o
3-MgO-TiO
2system's pottery, both maintained original dielectric loss and the little feature of temperature factor, its specific inductivity have also been obtained and significantly improves.Be widely used in the components and parts such as various electrical condenser, electricradiator, microwave device, ferroelectric memory device because having excellent piezoelectric and dielectric properties.
Embodiment 1: by atmosphere 300 DEG C dehydration 48h after KCl, NaCl and 150 DEG C of dry 24h after granularity be 100 object MgO, TiO
2kCl:NaCl:MgO:TiO in molar ratio
2=35:35:15:15 weighs and fully mixing, and mixing salt is put into corundum crucible; Electrified regulation is to 750 DEG C, and constant temperature pre-synthesis reacts 2h; After 150 DEG C of dry 24h, granularity is 100 order La
2o
3powder is by pre-synthesis reaction MgO, TiO
2the amount of powder is with mol ratio La
2o
3: MgO:TiO
2=2:49:49 weighs, by the La weighed
2o
3after powder is warming up to 950 DEG C after adding pre-synthesis system, constant temperature carries out whole building-up reactions 1h; With after distilled water cleaning reaction thing after system air cooling, its insoluble solid particle drying and obtain end product.Fused salt volatilization quality is 3%, and the recovery rate of powder is 95%, by material phase analysis, product is mainly (La, Mg)-and (Ti, La) O
6, mean particle size is 2um, meets (La, Mg)-(Ti, La) O
6it is the requirement of dielectric ceramic sintering powder.
Embodiment 2: by atmosphere 300 DEG C dehydration 48h after KCl, NaCl and 150 DEG C of dry 24h after granularity be 200 object MgO, TiO
2kCl:NaCl:MgO:TiO in molar ratio
2=25:25:25:25 weighs and fully mixing, and mixing salt is put into corundum crucible; Electrified regulation is to 850 DEG C, and constant temperature pre-synthesis reacts 4h; After 150 DEG C of dry 24h, granularity is 200 order La
2o
3powder is by pre-synthesis reaction MgO, TiO
2the amount of powder is with mol ratio La
2o
3: MgO:TiO
2=1:49.5:49.5 weighs, by the La weighed
2o
3after powder is warming up to 1050 DEG C after adding pre-synthesis system, constant temperature carries out whole building-up reactions 2h; With after distilled water cleaning reaction thing after system air cooling, its insoluble solid particle drying and obtain end product.Fused salt volatilization quality is 5%, and the recovery rate of powder is 96%, by material phase analysis, product is mainly (La, Mg)-and (Ti, La) O
6, mean particle size is 5um, meets (La, Mg)-(Ti, La) O
6it is the requirement of dielectric ceramic sintering powder.
Embodiment 3: by atmosphere 300 DEG C dehydration 48h after CaCl
2, granularity is 100 object MgO, TiO after NaCl and 150 DEG C dry 24h
2caCl in molar ratio
2: NaCl:MgO:TiO
2=35:35:15:15 weighs and fully mixing, and mixing salt is put into corundum crucible; Electrified regulation is to 750 DEG C, and constant temperature pre-synthesis reacts 2h; After 150 DEG C of dry 24h, granularity is 100 order La
2o
3powder is by pre-synthesis reaction MgO, TiO
2the amount of powder is with mol ratio La
2o
3: MgO:TiO
2=2:49:49 weighs, by the La weighed
2o
3after powder is warming up to 950 DEG C after adding pre-synthesis system, constant temperature carries out whole building-up reactions 1h; With after distilled water cleaning reaction thing after system air cooling, its insoluble solid particle drying and obtain end product.Fused salt volatilization quality is 3%, and the recovery rate of powder is 95%, by material phase analysis, product is mainly (La, Mg)-and (Ti, La) O
6, mean particle size is 2um, meets (La, Mg)-(Ti, La) O
6it is the requirement of dielectric ceramic sintering powder.
Embodiment 4: by atmosphere 300 DEG C dehydration 48h after CaCl
2, granularity is 300 object MgO, TiO after NaCl and 150 DEG C dry 24h
2caCl in molar ratio
2: NaCl:MgO:TiO
2=25:25:25:25 weighs and fully mixing, and mixing salt is put into corundum crucible; Electrified regulation is to 850 DEG C, and constant temperature pre-synthesis reacts 4h; After 150 DEG C of dry 24h, granularity is 200 order La
2o
3powder is by pre-synthesis reaction MgO, TiO
2the amount of powder is with mol ratio La
2o
3: MgO:TiO
2=1:49.5:49.5 weighs, by the La weighed
2o
3after powder is warming up to 1050 DEG C after adding pre-synthesis system, constant temperature carries out whole building-up reactions 2h; With after distilled water cleaning reaction thing after system air cooling, its insoluble solid particle drying and obtain end product.Fused salt volatilization quality is 5%, and the recovery rate of powder is 96%, by material phase analysis, product is mainly (La, Mg)-and (Ti, La) O
6, mean particle size is 5um, meets (La, Mg)-(Ti, La) O
6it is the requirement of dielectric ceramic sintering powder.
Embodiment 5: by atmosphere 300 DEG C dehydration 48h after CaCl
2, granularity is 100 object MgO, TiO after KCl and 150 DEG C dry 24h
2caCl in molar ratio
2: KCl:MgO:TiO
2=35:35:15:15 weighs and fully mixing, and mixing salt is put into corundum crucible; Electrified regulation is to 750 DEG C, and constant temperature pre-synthesis reacts 2h; After 150 DEG C of dry 24h, granularity is 100 order La
2o
3powder is by pre-synthesis reaction MgO, TiO
2the amount of powder is with mol ratio La
2o
3: MgO:TiO
2=2:49:49 weighs, by the La weighed
2o
3after powder is warming up to 950 DEG C after adding pre-synthesis system, constant temperature carries out whole building-up reactions 1h; With after distilled water cleaning reaction thing after system air cooling, its insoluble solid particle drying and obtain end product.Fused salt volatilization quality is 3%, and the recovery rate of powder is 95%, by material phase analysis, product is mainly (La, Mg)-and (Ti, La) O
6, mean particle size is 2um, meets (La, Mg)-(Ti, La) O
6it is the requirement of dielectric ceramic sintering powder.
Embodiment 6: by atmosphere 300 DEG C dehydration 48h after CaCl
2, granularity is 200 object MgO, TiO after KCl and 150 DEG C dry 24h
2caCl in molar ratio
2: KCl:MgO, TiO
2=25:25:25:25 weighs and fully mixing, and mixing salt is put into corundum crucible; Electrified regulation is to 850 DEG C, and constant temperature pre-synthesis reacts 4h; After 150 DEG C of dry 24h, granularity is 200 order La
2o
3powder is by pre-synthesis reaction MgO, TiO
2the amount of powder is with mol ratio La
2o
3: MgO:TiO
2=1:49.5:49.5 weighs, by the La weighed
2o
3after powder is warming up to 1050 DEG C after adding pre-synthesis system, constant temperature carries out whole building-up reactions 2h; With after distilled water cleaning reaction thing after system air cooling, its insoluble solid particle drying and obtain end product.Fused salt volatilization quality is 5%, and the recovery rate of powder is 96%, by material phase analysis, product is mainly (La, Mg)-and (Ti, La) O
6, mean particle size is 5um, meets (La, Mg)-(Ti, La) O
6it is the requirement of dielectric ceramic sintering powder.
Claims (6)
1. a molten-salt growth method synthesis La
2o
3-MgO-TiO
2be dielectric ceramic sintering powder, it is characterized in that: by KCl, NaCl, CaCl not containing crystal water
2in any two kinds of villaumites and not containing the granularity 100-200 object La of crystal water
2o
3, MgO, TiO
2oxide powder sintering forms; MgO, TiO
2it is 30 ~ 50% that mixture accounts for pre-synthesis reaction system material molar content, wherein MgO:TiO
2mol ratio is 1:1; KCl, NaCl, CaCl
2in any two kinds of villaumite mixtures to account for pre-synthesis reaction system material molar content be 50 ~ 70%, villaumite mixing mol ratio is 1:1; La
2o
3account for La
2o
3, MgO, TiO
2the molar content of material total amount is 1 ~ 2%.
2. a molten-salt growth method synthesis La
2o
3-MgO-TiO
2be dielectric ceramic sintering powder sintering method: it is characterized in that: comprise the following steps:
(1) proportioning starting material:
By KCl, NaCl, CaCl not containing crystal water
2in any two kinds of villaumites be the medium of building-up reactions, not containing the granularity 100-200 object La of crystal water
2o
3, MgO, TiO
2oxide powder is primitive reaction material;
Ratio requirement:
Pre-synthesis system: MgO, TiO
2it is 30 ~ 50% that mixture accounts for pre-synthesis reaction system material molar content, wherein MgO:TiO
2mol ratio is 1:1; KCl, NaCl, CaCl
2in any two kinds of villaumite mixtures to account for pre-synthesis reaction system material molar content be 50 ~ 70%, villaumite mixing mol ratio is 1:1;
Whole synthetic system: La
2o
3account for La
2o
3, MgO, TiO
2the molar content 1 ~ 2% of material total amount adds pre-synthesis system;
(2) pre-synthesis:
Abundant dewatered raw material, with MgO, TiO of above-mentioned steps (1) described content
2kCl, NaCl, CaCl of mixed oxide and mol ratio 1:1
2in villaumite, any two kinds of mixing salts fully mix, and load reactor, require to react 2-4h at temperature 750 ~ 850 DEG C;
(3) synthesis eventually:
System to pre-synthesis adds the La of above-mentioned steps (1) described content
2o
3, at temperature 950 ~ 1050 DEG C reaction 1-2h;
(4) collection of product:
After distilled water cleaning reaction thing, its insoluble solid particle drying and obtain end product-La
2o
3-MgO-TiO
2it is dielectric ceramic sintering powder.
3. a kind of molten-salt growth method synthesizes La according to claim 2
2o
3-MgO-TiO
2be dielectric ceramic sintering powder sintering method: it is characterized in that: not containing KCl, NaCl, CaCl of crystal water
2villaumite is by KCl, NaCl, the CaCl containing crystal water
2the villaumite 48h that dewaters at 300 DEG C of temperature in atmosphere obtains.
4. a kind of molten-salt growth method synthesizes La according to claim 2
2o
3-MgO-TiO
2be dielectric ceramic sintering powder sintering method: it is characterized in that: not containing the granularity 100-200 object La of crystal water
2o
3, MgO, TiO
2oxide powder is by granularity 100-200 object La
2o
3, MgO, TiO
2oxide powder in atmosphere at 150 DEG C of temperature dry 24h obtain.
5. a kind of molten-salt growth method synthesizes La according to claim 2
2o
3-MgO-TiO
2be dielectric ceramic sintering powder sintering method: it is characterized in that: pre-synthesis Reactive Synthesis temperature will make the substance system of set proportioning fully melt, the volatile quantity of fused salt is 3-5%.
6. a kind of molten-salt growth method synthesizes La according to claim 2
2o
3-MgO-TiO
2be dielectric ceramic sintering powder sintering method: it is characterized in that: Best Applying Condition: be 100 object MgO:TiO by granularity after KCl, NaCl after 300 DEG C of dehydration 48h in atmosphere and 150 DEG C of dry 24h
2kCl:NaCl:MgO:TiO in molar ratio
2=35:35:15:15 weighs and fully mixing, and mixing salt is put into corundum crucible; Electrified regulation is to 750 DEG C, and constant temperature pre-synthesis reacts 2h; After 150 DEG C of dry 24h, granularity is 100 order La
2o
3powder is by pre-synthesis reaction MgO:TiO
2the amount of powder is with mol ratio La
2o
3: MgO:TiO
2=2:49:49 weighs, by the La weighed
2o
3powder add with synthetic system after be warming up to 950 DEG C after constant temperature carry out whole building-up reactions 1h; With after distilled water cleaning reaction thing after system air cooling, its insoluble solid particle drying and obtain end product; Fused salt volatilization quality is 3%, and the recovery rate of powder is 95%.
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|---|---|---|---|---|
| CN108585795A (en) * | 2018-07-11 | 2018-09-28 | 中国科学院新疆理化技术研究所 | A kind of method that molten salt process prepares negative temperature coefficient thermal-sensitive ceramic material |
| CN114956175A (en) * | 2022-04-22 | 2022-08-30 | 中南大学 | Flake doped bismuth calcium niobate and preparation method and application thereof |
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| AIMIN YANG ET AL.: "Microwave Dielectric Properties of Low Temperature Cofired Glass-Ceramic Based on B2O3-La2O3-MgO-TiO2 Glass with La(Mg0.5Ti0.5)O3 Ceramics", 《JAPANESE JOURNAL OF APPLIED PHYSICS》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108585795A (en) * | 2018-07-11 | 2018-09-28 | 中国科学院新疆理化技术研究所 | A kind of method that molten salt process prepares negative temperature coefficient thermal-sensitive ceramic material |
| CN108585795B (en) * | 2018-07-11 | 2021-02-05 | 中国科学院新疆理化技术研究所 | Method for preparing negative temperature coefficient thermal sensitive ceramic material by salt melting method |
| CN114956175A (en) * | 2022-04-22 | 2022-08-30 | 中南大学 | Flake doped bismuth calcium niobate and preparation method and application thereof |
| CN114956175B (en) * | 2022-04-22 | 2023-09-08 | 中南大学 | Flaky doped bismuth calcium niobate and preparation method and application thereof |
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| CN104310992B (en) | 2016-03-30 |
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