CN106083026A - A kind of ultralow temperature molten salt preparation method of microwave dielectric nano-ceramic powder aluminic acid neodymium - Google Patents
A kind of ultralow temperature molten salt preparation method of microwave dielectric nano-ceramic powder aluminic acid neodymium Download PDFInfo
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Abstract
The present invention relates to the ultralow temperature molten salt preparation method of a kind of microwave dielectric nano-ceramic powder aluminic acid neodymium, belong to microwave dielectric material technical field.Nd (NO is weighed according to mol ratio 1: 1: 6～1: 1.1: 63)3·6H2O、Al(NO3)3·9H2O and KOH, load with zirconia balls be mill be situated between, in nylon tank with dehydrated alcohol as disperse medium, ball milling, drying；Be placed in alumina crucible, at 250～700 DEG C calcine 2～6h, wash, be dried i.e. can get the NdAlO that average grain size is about 100nm3Nano-powder.The equipment that the inventive method reaction temperature is low, energy consumption is low, need not costliness carries out producing and just can obtain the NdAlO that granular size is homogeneous, sintering activity is high3Nano material, it is possible to achieve large-scale production；And fused salt can wash removing with water and use through recrystallization Posterior circle, beneficially environmental protection.
Description
Technical field
The present invention relates to the ultralow temperature molten salt preparation method of a kind of microwave dielectric nano-ceramic powder aluminic acid neodymium, belong to microwave
Dielectric material technical field.
Background technology
Microwave dielectric ceramic materials is the novel electron ceramic material that fast development is got up in recent decades, mobile whole
The high-tech areas such as end, WLAN, Bluetooth technology, GPS technology, microwave communication base station, satellite television receiving system and military radar
Have a good application prospect.The wherein aluminic acid neodymium (NdAlO of perovskite structure3) pottery has suitable dielectric constant (εr=
22) and ultra-low loss (Q=5800), therefore, NdAlO3Pottery is a kind of microwave-medium ceramics material very with development potentiality
Material.Due to NdAlO3Pottery not only has good dielectric properties, also has fabulous lattice and thermal expansion matching, uses at present
Make the substrate material of dielectric resonator and high-temperature superconductor electronic devices and components to have obtained and be widely recognized as.
At present, in microwave electron ceramic industry, the preparation of aluminum base oxide functional material is widely used traditional pottery
Powder body process high-temperature solid phase calcination method, will form required thing phase through high-temperature calcination after oxide raw material mixing.The method
Middle solid state reaction mainly generates product nucleus on reactant crystal grain boundary or in the lattice neighbouring with interface, it is necessary to rely on high temperature
Advance ion diffusion and reconstruction.Wherein, conventional solid-state method synthesis NdAlO3The temperature of powder body is up to 1400 DEG C of (Journal
Of Materials Research, 1999 volume 14 page 114).The subject matter that conventional solid-state method exists is raw material particle size
Greatly (more than micron order), ball mill mixing is difficult to the homogenization accomplishing differential responses thing on molecular scale, because forming difficulty mutually.More
For it is important that the high-temperature calcination powder granule degree that causes synthetic product is big, generally also more than micron order, thus sintering activity
Difference, is difficulty with the system of high-compactness superfine ceramics (ceramic crystalline grain yardstick is at nanometer or submicron order) with it for precursor powder
Standby.Ceramic crystalline grain refinement is particularly significant for microwave electron pottery quality-improving.Relative to coarse-grain pottery, (ceramic crystalline grain yardstick exists
More than micron order), superfine ceramics, generally while strengthening ceramic body mechanical strength, also helps acquisition and shows based on dimensional effect
Write the electric property promoting material.In addition, it is accordingly required in particular to be concerned with superfine ceramics and can significantly reduce the chi of electronic devices and components
Very little, meet the high-end microwave electron ceramic component needs to miniaturization with integrated direction development.
Owing to precursor powder can affect the important physical properties (such as sintered density, piezoelectric property) of pottery, so, the most several
Year researchers efforts be made so that differently synthesis always, and chemical uniformity is good, narrow particle size distribution, form are controlled, good dispersion
NdAlO3Powder body.Up to the present, it is applied to NdAlO3The chemical method of powder body synthesis mainly has sol-gel process
(Journal of Sol-Gel Science and Technology, 2010 volume 53 page 227) and coprecipitation (material
Scientific and engineering journal, 2013 volume 31 page 380).But, there is use Organic substance, response time length, reaction in these methods
The problem such as temperature is of a relatively high and technological process is complicated.Therefore, find a kind of ultra low temperature, quick, technique is simple, environmental protection
NdAlO3Nano-powder synthetic method has great importance.
Molten-salt growth method is development in recent years a kind of chemical synthesis process faster.In the method, fused salt as reaction medium with
Reactant mixes, and the low viscosity liquid phase environment that fused salt is formed is conducive to accelerating the dissolving of reactant, mass transfer and forming core, generally can be in
In relatively low reaction temperatures and short period, synthesis conventional solid method is difficult to the pure phase oxide powder body obtained.Owing to fused salt generally selects
With water-soluble inorganic salt (such as KCl, NaCl, LiNO3, Na2SO4Deng), can be removed by simple water-washing step after having reacted
Obtain pure product.Additionally, the fused salt that washing removes can also use through re-crystallization cycles, be conducive to energy-saving and cost-reducing.Fused salt
Method synthesizer is simple, similar to solid phase method, it is easy to integrate with industry and carry out volume production.Famous American material scholar Stanislaus
S Wong claims molten-salt growth method to be based on Green Chemistry (Green Chemistry) in the survey article of its materials chemistry synthetic method
The environmentally benign synthesis of theory.But, yet there are no molten-salt growth method and prepare NdAlO3The relevant report of powder body.At ultralow temperature
Fused salt prepares NdAlO3In powder body, choosing of fused salt is most important.First one or more reactants are soluble in melted fused salt
In.Secondly the introduction of fused salt brings new impurity can not to whole reaction system, and easily removes.Raw material Nd2O3And Al2O3
Powder is insoluble in the water soluble chloride of generally selection, nitrate, sulfate etc., is soluble in KF salt.But, KF salt has play
Poison, all works the mischief to human body and environment in preparation process, which has limited molten-salt growth method and prepares NdAlO3The popularization of powder body.
Summary of the invention
The technology of the present invention solves problem: overcome the deficiencies in the prior art, proposes a kind of microwave-medium ceramics nano powder
The ultralow temperature molten salt preparation method of body aluminic acid neodymium.Raw material used by the method is Nd (NO3)3·6H2O、Al(NO3)3·9H2O and
KOH powder, is blended between raw material generation displacement reaction by mechanical mill and obtains highly active NdAlO3Presoma and nitrate,
Then the mixture obtained is calcined 2～6h at 250～700 DEG C, prepare NdAlO3Nano-powder.The method is a kind of green
Colour chemistry method, fused salt provides liquid phase environment for reaction system, is conducive to controlling product morphology and reducing synthesis temperature.Additionally,
The method technological process is simple, similar to solid phase method, it is easy to integrate with industry；And fused salt can wash removing with water after recrystallization
Recycle, beneficially environmental protection.NdAlO prepared by the present invention3Nano powder crystal particle scale is uniform, and reactivity is high.
The technical solution of the present invention is:
The ultralow temperature molten salt preparation method of a kind of microwave dielectric nano-ceramic powder aluminic acid neodymium, comprises the following steps:
(1) raw materials used it is: Nd (NO3)3·6H2O、Al(NO3)3·9H2O, KOH, wherein Nd (NO3)3·6H2O、Al
(NO3)3·9H2The mol ratio of O and KOH is 1: 1: 6～1: 1.1: 6, carries out weighing dispensing；
(2) dispensing of step (1) is loaded with zirconia balls be mill be situated between, nylon tank with dehydrated alcohol as disperse medium
In carry out ball milling, the rotating speed of ball milling is 100～400r/min, and Ball-milling Time is 6～24h；
(3) ball mill mixing of step (2) being dried process, baking temperature is 80～150 DEG C, drying time be 4～
8h；
(4) batch mixing of step (3) dried is positioned in alumina crucible, seals, calcine at 250～700 DEG C,
Temperature retention time is 2～6h；
(5) powder body obtaining step (4) carries out deionized water centrifuge washing, removes fused salt, the most i.e. obtains aluminic acid neodymium
Nano-powder.
Reaction equation is:
Compared with prior art, the invention have the advantages that
(1) present invention is first with Nd (NO3)3·6H2O、Al(NO3)3·9H2O and KOH powder is raw material, through weighing,
Mechanical mill mixing occur displacement reaction, be dried, ionic reaction, centrifuge washing obtain NdAlO under fused salt liquid phase environment3Nano powder
Body.Show through analyzing, NdAlO3Nano-powder crystal particle scale is uniform, crystallite dimension is about 100nm, sintering activity is high, for relatively
The ceramic sintered bodies preparing densification under low temperature provides possibility.
(2) the microwave dielectric material NdAlO that the present invention provides3In the preparation method of nano-powder ultralow temperature, fused salt provides
Liquid phase environment advantageously reduce synthesis temperature, thus high-purity NdAlO can be obtained ultralow temperature 250～700 DEG C3Nano powder
Body.
(3) the fused salt potassium nitrate that the present invention uses is by raw material Nd (NO3)3·6H2O、Al(NO3)3·9H2O, KOH machinery
The displacement reaction gained of mixing induction, nontoxic, tasteless, human body will not be damaged.
(4) the microwave dielectric material NdAlO that the present invention provides3The preparation method technique of nano-powder ultralow temperature is simple, system
The standby cycle is short, energy consumption and low cost, it is easy to accomplish, there is stronger practicality.
(5) the ultralow temperature molten salt preparation method of a kind of microwave dielectric nano-ceramic powder aluminic acid neodymium, belongs to microwave-medium material
Material technical field.Nd (NO is weighed according to mol ratio 1: 1: 6～1: 1.1: 63)3·6H2O、Al(NO3)3·9H2O and KOH, loads
With zirconia balls be mill be situated between, in nylon tank with dehydrated alcohol as disperse medium, ball milling, drying；It is placed in alumina crucible,
At 250～700 DEG C calcine 2～6h, wash, be dried i.e. can get the NdAlO that average grain size is about 100nm3Nano powder
Body.The inventive method reaction temperature is low, energy consumption is low, need not the equipment of costliness carries out producing that just can to obtain granular size equal
One, the NdAlO that sintering activity is high3Nano material, it is possible to achieve large-scale production；And fused salt can wash removing with water through recrystallization
Posterior circle uses, beneficially environmental protection.
Accompanying drawing explanation
Use Bruker Advance D-8 powder x ray diffractometer x (Cu KαRadiation,) measure made
The X-ray diffractogram of standby material.The microstructure preparing material is saturating by Apollo300 scanning electron microscope and Tecnai F20
Penetrate ultramicroscope to be measured.
Fig. 1 is the X ray diffracting spectrum of mechanical ball milling batch mixing prepared by the present invention.
Fig. 2 is NdAlO prepared by the present invention3The X ray diffracting spectrum of nano-powder, wherein, curve a～f respectively presses
According to the NdAlO obtained by embodiment 1～63The X ray diffracting spectrum of nano-powder.
NdAlO prepared by Fig. 3 present invention3The scanning electron microscope (SEM) photograph of nano-powder.
NdAlO prepared by Fig. 4 present invention3The transmission electron microscope picture of nano-powder and high-resolution Fourier transformation figure.
Detailed description of the invention
The ultralow temperature molten salt preparation method of a kind of microwave dielectric nano-ceramic powder aluminic acid neodymium, comprises the following steps:
(1) raw materials used it is: Nd (NO3)3·6H2O、Al(NO3)3·9H2O, KOH, wherein Nd (NO3)3·6H2O、Al
(NO3)3·9H2The mol ratio of O and KOH is 1: 1: 6～1: 1.1: 6, carries out weighing dispensing；
(2) dispensing of step (1) is loaded with zirconia balls be mill be situated between, nylon tank with dehydrated alcohol as disperse medium
In carry out ball milling, the rotating speed of ball milling is 100～400r/min, and Ball-milling Time is 6～24h；
(3) ball mill mixing of step (2) being dried process, baking temperature is 80～150 DEG C, drying time be 4～
8h；
(4) batch mixing of step (3) dried is positioned in alumina crucible, seals, calcine at 250～700 DEG C,
Temperature retention time is 2～6h；
(5) powder body obtaining step (4) carries out deionized water centrifuge washing, removes fused salt, the most i.e. obtains aluminic acid neodymium
Nano-powder.
The invention will be further described with embodiment below in conjunction with the accompanying drawings.
Embodiment 1
(1) raw materials used it is: Nd (NO3)3·6H2O、Al(NO3)3·9H2O, KOH, wherein Nd (NO3)3·6H2O、Al
(NO3)3·9H2The mol ratio of O and KOH is 1: 1: 6, carries out weighing dispensing；
(2) dispensing of step (1) is loaded with zirconia balls be mill be situated between, nylon tank with dehydrated alcohol as disperse medium
In carry out ball milling, the rotating speed of ball milling is 200r/min, and Ball-milling Time is 12h；
(3) ball mill mixing of step (2) being dried process, baking temperature is 80 DEG C, and drying time is 8h；
(4) batch mixing of step (3) dried is positioned in alumina crucible, seals, calcine at 250 DEG C, insulation
Time is 4h；
(5) powder body obtaining step (4) carries out deionized water centrifuge washing, removes fused salt, the most i.e. obtains NdAlO3
Nano-powder a.
Experiment shows: in the ball mill mixing stage, and mechanical mixture causes there occurs between raw material displacement reaction, and KNO3For only
One amorphous material showed in XRD, the presoma such as neodymium and aluminum is then to exist with amorphous phase.The KNO generated3Play molten
The effect of salt assitant.Although presoma crystallinity is poor, but amorphous substance reactivity is high, may advantageously facilitate NdAlO3At nitre
Hydrochlorate generates (ball mill mixing x-ray diffractogram of powder spectrum is shown in Fig. 1).Gained NdAlO3Nano-powder is pure perovskite phase structure
(x-ray diffractogram of powder spectrum is shown in Fig. 2), crystal grain presents cube pattern and size is uniform, and average grain size is about 100nm
(powder stereoscan photograph is shown in that Fig. 3, powder transmission electron microscope photo are shown in Fig. 4).Remaining embodiment gained NdAlO3Nano-powder is equal
There is pure perovskite phase structure and similar grain morphology, and average grain size is about 100nm～150nm.
Embodiment 2
(1) raw materials used it is: Nd (NO3)3·6H2O、Al(NO3)3·9H2O, KOH, wherein Nd (NO3)3·6H2O、Al
(NO3)3·9H2The mol ratio of O and KOH is 1: 1.02: 6, carries out weighing dispensing；
(2) dispensing of step (1) is loaded with zirconia balls be mill be situated between, nylon tank with dehydrated alcohol as disperse medium
In carry out ball milling, the rotating speed of ball milling is 100r/min, and Ball-milling Time is 24h；
(3) ball mill mixing of step (2) being dried process, baking temperature is 100 DEG C, and drying time is 6h；
(4) batch mixing of step (3) dried is positioned in alumina crucible, seals, calcine at 300 DEG C, insulation
Time is 3h；
(5) powder body obtaining step (4) carries out deionized water centrifuge washing, removes fused salt, the most i.e. obtains NdAlO3
Nano-powder b.The x-ray diffractogram of powder spectrum of product b is shown in Fig. 2.
Embodiment 3
(1) raw materials used it is: Nd (NO3)3·6H2O、Al(NO3)3·9H2O, KOH, wherein Nd (NO3)3·6H2O、Al
(NO3)3·9H2The mol ratio of O and KOH is 1: 1.04: 6, carries out weighing dispensing；
(2) dispensing of step (1) is loaded with zirconia balls be mill be situated between, nylon tank with dehydrated alcohol as disperse medium
In carry out ball milling, the rotating speed of ball milling is 300r/min, and Ball-milling Time is 8h；
(3) ball mill mixing of step (2) being dried process, baking temperature is 120 DEG C, and drying time is 5h；
(4) batch mixing of step (3) dried is positioned in alumina crucible, seals, calcine at 400 DEG C, insulation
Time is 5h；
(5) powder body obtaining step (4) carries out deionized water centrifuge washing, removes fused salt, the most i.e. obtains NdAlO3
Nano-powder c.The x-ray diffractogram of powder spectrum of product c is shown in Fig. 2.
Embodiment 4
(1) raw materials used it is: Nd (NO3)3·6H2O、Al(NO3)3·9H2O, KOH, wherein Nd (NO3)3·6H2O、Al
(NO3)3·9H2The mol ratio of O and KOH is 1: 1.06: 6, carries out weighing dispensing；
(2) dispensing of step (1) is loaded with zirconia balls be mill be situated between, nylon tank with dehydrated alcohol as disperse medium
In carry out ball milling, the rotating speed of ball milling is 400r/min, and Ball-milling Time is 6h；
(3) ball mill mixing of step (2) being dried process, baking temperature is 150 DEG C, and drying time is 4h；
(4) batch mixing of step (3) dried is positioned in alumina crucible, seals, calcine at 500 DEG C, insulation
Time is 6h；
(5) powder body obtaining step (4) carries out deionized water centrifuge washing, removes fused salt, the most i.e. obtains NdAlO3
Nano-powder d.The x-ray diffractogram of powder spectrum of product d is shown in Fig. 2.
Embodiment 5
(1) raw materials used it is: Nd (NO3)3·6H2O、Al(NO3)3·9H2O, KOH, wherein Nd (NO3)3·6H2O、Al
(NO3)3·9H2The mol ratio of O and KOH is 1: 1.08: 6, carries out weighing dispensing；
(2) dispensing of step (1) is loaded with zirconia balls be mill be situated between, nylon with dehydrated alcohol as disperse medium
Carrying out ball milling in tank, the rotating speed of ball milling is 400r/min, and Ball-milling Time is 8h；
(3) ball mill mixing of step (2) being dried process, baking temperature is 100 DEG C, and drying time is 5h；
(4) batch mixing of step (3) dried is positioned in alumina crucible, seals, calcine at 600 DEG C, insulation
Time is 2h；
(5) powder body obtaining step (4) carries out deionized water centrifuge washing, removes fused salt, the most i.e. obtains NdAlO3
Nano-powder e.The x-ray diffractogram of powder spectrum of product e is shown in Fig. 2.
Embodiment 6
(1) raw materials used it is: Nd (NO3)3·6H2O、Al(NO3)3·9H2O, KOH, wherein Nd (NO3)3·6H2O、Al
(NO3)3·9H2The mol ratio of O and KOH is 1: 1.1: 6, carries out weighing dispensing；
(2) dispensing of step (1) is loaded with zirconia balls be mill be situated between, nylon tank with dehydrated alcohol as disperse medium
In carry out ball milling, the rotating speed of ball milling is 400r/min, and Ball-milling Time is 12h；
(3) ball mill mixing of step (2) being dried process, baking temperature is 120 DEG C, and drying time is 4h；
(4) batch mixing of step (3) dried is positioned in alumina crucible, seals, calcine at 700 DEG C, insulation
Time is 3h；
(5) powder body obtaining step (4) carries out deionized water centrifuge washing, removes fused salt, the most i.e. obtains NdAlO3
Nano-powder f.The x-ray diffractogram of powder spectrum of product f is shown in Fig. 2.
NdAlO prepared by the various embodiments described above3The X ray diffracting spectrum of nano-powder is shown in Fig. 2, as can be seen from the figure
Powder body prepared by each embodiment is pure perovskite phase structure, produces without the second phase.The scanning electron microscope of powder body and transmission electron microscope
Photo is shown in that Fig. 3 and Fig. 4, powder grain present cube pattern, and average grain size is about 100nm.
Claims (9)
1. the ultralow temperature molten salt preparation method of a nano-powder aluminic acid neodymium, it is characterised in that comprise the following steps:
(1) by Nd (NO3)3·6H2O、Al(NO3)3·9H2O and KOH carries out ball milling, obtains batch mixing；
(2) batch mixing obtained after step (1) ball milling is dried process；
(3) batch mixing after step (2) dried is calcined；
(4) batch mixing after step (3) being calcined uses deionized water to be centrifuged washing, obtains aluminic acid neodymium nano powder after drying
Body.
The ultralow temperature molten salt preparation method of a kind of nano-powder aluminic acid neodymium the most according to claim 1, it is characterised in that: institute
State Nd (NO in step (1)3)3·6H2O、Al(NO3)3·9H2The mol ratio of O, KOH is 1: 1: 6～1: 1.1: 6.
The ultralow temperature molten salt preparation method of a kind of nano-powder aluminic acid neodymium the most according to claim 1, it is characterised in that: institute
State and be situated between for mill with zirconia balls when step (1) carries out ball milling.
The ultralow temperature molten salt preparation method of a kind of nano-powder aluminic acid neodymium the most according to claim 1, it is characterised in that: institute
State when step (1) carries out ball milling with dehydrated alcohol as disperse medium.
The ultralow temperature molten salt preparation method of a kind of nano-powder aluminic acid neodymium the most according to claim 1, it is characterised in that: institute
Stating the ball grinder carrying out in step (1) being used during ball milling is nylon tank.
6. carrying out the rotating speed of ball milling during ball milling is 100～400r/min, and Ball-milling Time is 6～24h.
The ultralow temperature molten salt preparation method of a kind of nano-powder aluminic acid neodymium the most according to claim 1, it is characterised in that: institute
Stating baking temperature in step (2) is 80～150 DEG C, and drying time is 4～8h.
The ultralow temperature molten salt preparation method of a kind of nano-powder aluminic acid neodymium the most according to claim 1, it is characterised in that: institute
State and carry out in alumina crucible when batch mixing is calcined by step (3), and alumina crucible is sealed.
The ultralow temperature molten salt preparation method of a kind of nano-powder aluminic acid neodymium the most according to claim 1, it is characterised in that: institute
Stating calcining heat in step (3) is 250～700 DEG C, and calcination time is 2～6h.
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|---|---|---|---|---|
| CN110563035A (en) * | 2019-10-14 | 2019-12-13 | 西北工业大学深圳研究院 | Rare earth zirconate nano powder and preparation method and application thereof |
| CN110627495A (en) * | 2019-09-23 | 2019-12-31 | 航天材料及工艺研究所 | Low-thermal-conductivity high-entropy aluminate ceramic and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102874870A (en) * | 2012-10-22 | 2013-01-16 | 北京工业大学 | Method for preparing LaAlO3-BiAlO3 snowflake-shaped nano powder at low temperature |
| US8902115B1 (en) * | 2010-07-27 | 2014-12-02 | Sandia Corporation | Resonant dielectric metamaterials |
| CN105000884A (en) * | 2015-08-18 | 2015-10-28 | 广东国华新材料科技股份有限公司 | Microwave dielectric ceramic material as well as preparation method and application thereof |
-
2016
- 2016-06-17 CN CN201610438977.0A patent/CN106083026A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8902115B1 (en) * | 2010-07-27 | 2014-12-02 | Sandia Corporation | Resonant dielectric metamaterials |
| CN102874870A (en) * | 2012-10-22 | 2013-01-16 | 北京工业大学 | Method for preparing LaAlO3-BiAlO3 snowflake-shaped nano powder at low temperature |
| CN105000884A (en) * | 2015-08-18 | 2015-10-28 | 广东国华新材料科技股份有限公司 | Microwave dielectric ceramic material as well as preparation method and application thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110627495A (en) * | 2019-09-23 | 2019-12-31 | 航天材料及工艺研究所 | Low-thermal-conductivity high-entropy aluminate ceramic and preparation method thereof |
| CN110627495B (en) * | 2019-09-23 | 2021-09-03 | 航天材料及工艺研究所 | Low-thermal-conductivity high-entropy aluminate ceramic and preparation method thereof |
| CN110563035A (en) * | 2019-10-14 | 2019-12-13 | 西北工业大学深圳研究院 | Rare earth zirconate nano powder and preparation method and application thereof |
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