CN115520898A - Preparation method and application of flaky microcrystalline powder - Google Patents
Preparation method and application of flaky microcrystalline powder Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title abstract description 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 36
- 150000003839 salts Chemical class 0.000 claims abstract description 29
- 239000002994 raw material Substances 0.000 claims abstract description 23
- 239000000919 ceramic Substances 0.000 claims abstract description 16
- 239000011780 sodium chloride Substances 0.000 claims abstract description 16
- 239000011521 glass Substances 0.000 claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000002243 precursor Substances 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
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- 230000008018 melting Effects 0.000 claims description 3
- BUKHSQBUKZIMLB-UHFFFAOYSA-L potassium;sodium;dichloride Chemical compound [Na+].[Cl-].[Cl-].[K+] BUKHSQBUKZIMLB-UHFFFAOYSA-L 0.000 claims description 2
- 239000013078 crystal Substances 0.000 abstract description 10
- 239000005385 borate glass Substances 0.000 abstract description 4
- 239000011777 magnesium Substances 0.000 description 55
- 239000012071 phase Substances 0.000 description 12
- 238000001144 powder X-ray diffraction data Methods 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 7
- 238000003746 solid phase reaction Methods 0.000 description 7
- 238000003786 synthesis reaction Methods 0.000 description 7
- 239000003989 dielectric material Substances 0.000 description 6
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- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 4
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- 229910010293 ceramic material Inorganic materials 0.000 description 4
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- 238000005516 engineering process Methods 0.000 description 4
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- 238000001308 synthesis method Methods 0.000 description 3
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 2
- 238000003780 insertion Methods 0.000 description 2
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- 239000013558 reference substance Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- OHVLMTFVQDZYHP-UHFFFAOYSA-N 1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-2-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound N1N=NC=2CN(CCC=21)C(CN1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)=O OHVLMTFVQDZYHP-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
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- C01G35/006—Compounds containing, besides tantalum, two or more other elements, with the exception of oxygen or hydrogen
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Abstract
The invention discloses a preparation method and application of flaky microcrystalline powder. The chemical general formula of the flaky microcrystalline powder is (Mg) 1‑x Zn x ) 4 (Ta 1‑y Nb y ) 2 O 9 Wherein x =0 to 1, y =0 to 1. The preparation method comprises the following steps: weighing raw materials according to a chemical formula, and weighing NaCl and KCl raw materials; grinding and uniformly mixing the raw materials and absolute ethyl alcohol, drying, and sintering in a muffle furnace at 950 ℃; grinding the sintered sample to be crushed, transferring the crushed sintered sample to a glass cup, adding deionized water, removing NaCl and KCl fused salt by heating, stirring, dissolving and filtering, and finally drying to obtain the flaky microcrystalline powder. The flaky microcrystalline powder has obvious crystal grain orientation, the radial length of 0.1-2.5 mu m, the thickness of 0.05-0.3 mu m and large aspect ratio. Can be used as precursor powder for producing microwave dielectric ceramics, scintillating transparent ceramics, borate glass microcrystalline scintillators, etc.
Description
Technical Field
The invention relates to a preparation method and application of flaky microcrystalline powder, belonging to the technical field of preparation processes of microwave dielectric materials and scintillation luminescent materials.
Background
Microwave dielectric ceramics, as a novel electronic material, are used as resonators, filters, dielectric substrates, dielectric antennas, dielectric waveguide loops and the like in modern communications, and are widely applied to many fields of microwave technology, such as mobile communications, television satellite receivers, satellite broadcasting, radars, radio remote control and the like. The high dielectric constant of the microwave dielectric ceramic material is beneficial to the miniaturization of the microwave dielectric filter, and the filter can realize the mixing and integration of a microwave circuit together with a microwave tube and a microstrip line, so that the size of a device reaches the millimeter level, and the price of the microwave dielectric ceramic material is much lower than that of a metal resonant cavity. If the resonant frequency of the microwave dielectric material is greatly changed along with the temperature, the carrier signal of the filter can drift at different temperatures, thereby affecting the use performance of the equipment. This requires that the resonant frequency of the material not vary too much with temperature. The actual desired range of temperature is approximately-40 deg.C to 100 deg.C, within which the material has a temperature coefficient of frequency of no greater than 10 ppm/deg.C. The dielectric loss of the microwave dielectric material is a main factor affecting the insertion loss of the dielectric filter. The Q value of the microwave dielectric material is in inverse proportion to the dielectric loss tan delta. The larger the Q value, the lower the insertion loss of the filter. A variety of microwave dielectric materials have been developed, including CaTiO 3 ，Ba(Zn 1/3 Ta 2/3 )O 6 、Mg 2 SiO 4 、Mg 4 Ta 2 O 9 And Mg 4 Nb 2 O 9 And the like. In order to improve the polarization efficiency and dielectric property of microwave dielectric material, namely to improve the dielectric constant andthe dielectric loss is reduced, the strength and the toughness of the ceramic material are improved, the flaky microcrystalline powder with better directionality is required to be used as a sintering raw material for sintering to prepare compact texture ceramic, and the technology becomes one of important technologies for preparing microwave dielectric ceramic materials with high dielectric property.
Mg 4 Ta 2 O 9 CdWO of crystal light yield and afterglow size and wide application in container security inspection 4 The crystals are close to each other, and the non-toxic elements, the energy resolution and the decay time of the crystals are less than those of CdWO 4 The crystal is made into a novel scintillation crystal material for the security inspection application of the container. Preliminary studies show that the optical yield can be obviously improved by doping Zn or Nb or Zn/Nb codoping, and the improvement of the optical yield leads the image definition to be increased, thereby being more beneficial to the application of the optical yield in the field of container security inspection. (Mg) 1-x Zn x ) 4 (Ta 1- y Nb y ) 2 O 9 Flaky microcrystalline powder in novel glass microcrystalline scintillator Li 2 B 4 O 7 -(Mg 1-x Zn x ) 4 (Ta 1-y Nb y ) 2 O 9 Has potential value in the aspect of performance optimization. Can be used for modulating and optimizing the scintillation luminescence property of the glass microcrystal. Larger particles (Mg) than those synthesized by solid phase sintering 1-x Zn x ) 4 (Ta 1-y Nb y ) 2 O 9 Spherical micron powder and flaky microcrystal doping have better luminous advantages.
However, currently synthesized by solid phase sintering (Mg) 1-x Zn x ) 4 (Ta 1-y Nb y ) 2 O 9 The synthesis temperature of the spherical micron powder is up to 1350 ℃, so that MgO and ZnO volatilize at the high temperature of more than 1300 ℃, the stoichiometric ratio is changed, and the crystal has impurity phases, so that when the spherical micron powder is used as precursor powder of a microwave dielectric ceramic, a scintillating transparent ceramic or a borate glass scintillator, the performance requirement can not be well met, and the application of the spherical micron powder is limited.
Disclosure of Invention
The purpose of the invention is: aiming at the prior MgO and ZnO solid phase sintering at high temperature (>1300 ℃) is easy to volatilize to cause the problem of impure phase, provides a method for preparing flaky microcrystalline powder at low temperature, and MgO, znO and Ta are used for preparing flaky microcrystalline powder 2 O 5 、Nb 2 O 5 Is a precursor and is subjected to topological melting reaction with NaCl and KCl in a molten salt system of NaCl and KCl to prepare (Mg) 1-x Zn x ) 4 (Ta 1-y Nb y ) 2 O 9 (x =0 to 1, y =0 to 1) a flaky microcrystalline powder. Powder XRD analysis shows that the powder is pure phase, and SEM test shows that the powder has obvious grain orientation, radial length of 0.5-2.5 micron and thickness of 0.05-0.3 micron. Having a large aspect ratio. Is an ideal template grain suitable for the Template Grain Growth (TGG) technology, namely a flaky microcrystal. Can be used for manufacturing (Mg) 1-x Zn x ) 4 (Ta 1-y Nb y ) 2 O 9 Precursor powders of microwave dielectric ceramics, scintillating transparent ceramics, borate glass scintillators, and the like.
In order to achieve the above object, the present invention provides a flaky microcrystalline powder having a chemical formula of (Mg) 1-x Zn x ) 4 (Ta 1-y Nb y ) 2 O 9 Wherein x =0 to 1, y =0 to 1, and the flaky microcrystalline powder has a crystal grain orientation, is flaky as shown in an SEM picture, and is formed by MgO, znO and Ta 2 O 5 、Nb 2 O 5 Is prepared by taking a precursor raw material and carrying out topological melting reaction in a NaCl-KCl molten salt system.
Preferably, the radial length of the flaky microcrystalline powder is 0.1-2.5 μm, and the thickness of the flaky microcrystalline powder is 0.05-0.3 μm.
The invention also provides a preparation method of the flaky microcrystalline powder, which comprises the following steps: weighing precursor raw materials MgO, znO and Ta according to a chemical general formula and a stoichiometric ratio 2 O 5 And Nb 2 O 5 And weighing NaCl and KCl raw materials, grinding and uniformly mixing the raw materials with absolute ethyl alcohol, drying, sintering at 950 ℃ in a muffle furnace, grinding a sintered sample until the sintered sample is crushed, transferring the crushed sintered sample to a container, adding deionized water, removing NaCl and KCl fused salt by adopting a heating, stirring, dissolving and suction filtering method, and finally drying to obtain the flaky microcrystalline powder.
Preferably, the ratio of the sum of the mass of the raw materials of NaCl and KCl to the sum of the mass of the raw materials of each precursor is 7:3.
preferably, the molar ratio of NaCl to KCl is 4:6 or 2:8.
preferably, the temperature rise rate of the sintering is 80-120 ℃/h, and the time is 1-2 h.
The invention also provides the application of the flaky microcrystalline powder in microwave dielectric ceramics, scintillating transparent ceramics or glass microcrystalline scintillators.
The present invention provides a molten salt method for synthesizing (Mg) at lower temp 1-x Zn x ) 4 (Ta 1-y Nb y ) 2 O 9 (x = 0-1, y = 0-1) and the synthesis temperature is 950 ℃, compared with 1350 ℃ of solid phase reaction, the flaky microcrystalline powder can avoid the volatilization of MgO and ZnO at the high temperature of 1300 ℃ and avoid the appearance of impure phases. Can be used for manufacturing (Mg) 1-x Zn x ) 4 (Ta 1-y Nb y ) 2 O 9 Precursor powder of microwave dielectric ceramic, scintillating transparent ceramic, borate glass microcrystal scintillator, etc.
Compared with the prior art, the invention has the beneficial effects that:
(1) The invention synthesizes (Mg) for the first time 1-x Zn x ) 4 (Ta 1-y Nb y ) 2 O 9 The flaky microcrystal powder has strong orientation and large aspect ratio, has the advantages of radial length of 0.5-2.5 mu m, thickness of 0.05-0.3 mu m and moderate size, is an ideal template crystal grain and can be used for manufacturing (Mg) 1-x Zn x ) 4 (Ta 1-y Nb y ) 2 O 9 The precursor powder of the compact microwave dielectric ceramic, the transparent scintillating ceramic with high transmittance and the glass microcrystal scintillator with high dielectric property, high toughness and high strength;
(2) Of the present invention (Mg) 1-x Zn x ) 4 (Ta 1-y Nb y ) 2 O 9 The synthesis temperature is 950 ℃, which is reduced by more than 300 ℃ compared with the synthesis temperature of about 1300 ℃ of solid phase sintering, and avoidsThe volatilization of MgO and ZnO during high-temperature synthesis can be maintained, the stoichiometric ratio of components and the like in the synthesis process can be kept unchanged, and the appearance of crystal impurity phases is avoided.
Drawings
FIG. 1 shows (Mg) prepared in each example 1-x Zn x ) 4 (Ta 1-y Nb y ) 2 O 9 X-ray diffraction pattern of flaky microcrystalline powder: (a) Solid phase reaction synthesized Mg 4 Ta 2 O 9 A powder reference substance; (b) Mg synthesized by molten salt method 4 Ta 2 O 9 Powder; (c) Mg synthesized by molten salt method 2 Zn 2 Ta 2 O 9 Powder; (d) Mg synthesized by molten salt method 4 TaNbO 9 Powder; (e) Mg synthesized by molten salt method 2 Zn 2 TaNbO 9 Powder; (f) Mg (magnesium) 4 Ta 2 O 9 -PDF#38-1458；
FIG. 2 is a solid phase reaction for the synthesis of Mg 4 Ta 2 O 9 SEM photograph of micron powder reference substance;
FIG. 3 is Mg prepared in example 1 4 Ta 2 O 9 SEM photograph of flaky microcrystalline powder;
FIG. 4 is Mg prepared in example 2 2 Zn 2 Ta 2 O 9 SEM photograph of flaky microcrystalline powder;
FIG. 5 is Mg prepared in example 3 4 TaNbO 9 SEM photograph of flaky microcrystalline powder;
FIG. 6 is Mg prepared in example 4 2 Zn 2 TaNbO 9 SEM photograph of the flaky microcrystalline powder.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
Example 1
According to Mg 4 Ta 2 O 9 The reaction equation of (1) is calculated, and 8.0199g of MgO (99.99%) and Ta are accurately weighed 2 O 5 (99.99%) 21.9801g, naCl (100%) 24.0317g, KCl (100%) 45.9683g, mixing each raw material with 50mL of absolute ethanol, grinding and mixing in agate mortar 4And h, transferring the mixture into a glass container for drying. Sieving the dried raw material, and adding Al 2 O 3 And covering the crucible, and sintering in a muffle furnace at 950 ℃ for 1h at a heating and cooling rate of 100 ℃/h. Grinding the sintered sample to be crushed, transferring the crushed sintered sample to a glass cup, adding deionized water, heating the crushed sintered sample to 75 ℃ in a water bath, magnetically stirring the crushed sintered sample for 20min, performing suction filtration for 10 times to remove NaCl and KCl fused salt in the crushed sintered sample, and drying the crushed sintered sample at 80 ℃ for 8h to obtain a powder sample. FIG. 1 (b) shows Mg synthesized by a molten salt method 4 Ta 2 O 9 Powder XRD pattern, and Mg 4 Ta 2 O 9 The diffraction peaks of the PDF standard card (FIG. 1 (f)) #38-1458 are in one-to-one correspondence, which indicates that the powder synthesized by the molten salt method is pure Mg 4 Ta 2 O 9 And (4) phase(s). Mg prepared by solid-phase reaction synthesis method 4 Ta 2 O 9 As is clear from the powder XRD pattern, i.e., from comparison with fig. 1 (a), the relative intensity of the (104) diffraction peak is enhanced, and the orientation is strong. The SEM photograph is shown in FIG. 3, from which it can be seen that Mg was synthesized by the molten salt method 4 Ta 2 O 9 Is sheet-shaped, has the radial length of 1 to 2.5 mu m and the thickness of 0.1 to 0.3 mu m, and has larger aspect ratio. In sharp contrast thereto, mg synthesized by solid phase reaction 4 Ta 2 O 9 The powder was approximately spherical, and had a particle size of 1 to 2.5 μm as shown in FIG. 2.
Example 2
According to Mg 2 Zn 2 Ta 2 O 9 3.5289g of MgO (99.99%), 7.1278g of ZnO (99.99%), and Ta were accurately weighed 2 O 5 (99.99%) 19.3433g, naCl (100%) 11.4738g, KCl (100%) 58.5262g, each raw material and 50mL of absolute ethanol are ground and mixed uniformly in an agate mortar for 4h, and the mixture is transferred to a glass container to be dried. Sieving the dried raw materials, and adding Al 2 O 3 The crucible is covered and sintered for 1h at 950 ℃ in a muffle furnace, and the heating and cooling rate is 100 ℃/h. Grinding the sintered sample to be crushed, transferring the crushed sintered sample to a glass cup, adding deionized water, heating the crushed sintered sample to 75 ℃ in a water bath, magnetically stirring the crushed sintered sample for 20min, performing suction filtration for 10 times to remove NaCl and KCl fused salt in the crushed sintered sample, and drying the crushed sintered sample at 80 ℃ for 8h to obtain a powder sample. FIG. 1 (c) shows Mg synthesized by a molten salt method 2 Zn 2 Ta 2 O 9 Powder XRD pattern, and Mg 4 Ta 2 O 9 The diffraction peaks of the PDF standard card (FIG. 1 (f)) #38-1458 of (A) are in one-to-one correspondence, and no impurity phase peak exists, which indicates that the powder synthesized by the molten salt method is a pure phase. Mg prepared by solid phase reaction synthesis method 4 Ta 2 O 9 As is clear from the powder XRD pattern, i.e., from comparison with fig. 1 (a), the relative intensity of the (104) diffraction peak is enhanced, and the orientation is further enhanced. The SEM photograph is shown in FIG. 4, from which it can be seen that Mg was synthesized by the molten salt method 2 Zn 2 Ta 2 O 9 The sheet-shaped material has a radial length of 1-2 μm and a thickness of 0.05-0.2 μm, and has a large aspect ratio.
Example 3
According to Mg 4 TaNbO 9 The reaction equation of (1) was calculated, and 9.3903g of MgO (99.99%) and Ta were weighed accurately 2 O 5 (99.99％)12.8680g、Nb 2 O 5 (99.99%) 7.7417g, naCl (100%) 24.0317g and KCl (100%) 45.9683g, mixing each raw material with 50mL of absolute ethyl alcohol, grinding and mixing uniformly in an agate mortar for 4h, transferring to a glass container and drying. Sieving the dried raw materials, and adding Al 2 O 3 And covering the crucible, and sintering in a muffle furnace at 950 ℃ for 1h at a heating and cooling rate of 100 ℃/h. Grinding the sintered sample to be crushed, transferring the crushed sintered sample to a glass cup, adding deionized water, heating the mixture in a water bath to 75 ℃, magnetically stirring the mixture for 20min, performing suction filtration for 10 times to remove NaCl and KCl fused salt in the mixture, and drying the mixture at 80 ℃ for 8h to obtain a powder sample. FIG. 1 (d) shows Mg synthesized by the molten salt method 4 TaNbO 9 Powder XRD pattern, and Mg 4 Ta 2 O 9 The diffraction peaks of the PDF standard card (figure 1 (f)) #38-1458 are in one-to-one correspondence, and no impurity phase peak exists, which indicates that the powder synthesized by the molten salt method is a pure phase. Mg prepared by solid phase reaction synthesis method 4 Ta 2 O 9 As is clear from the powder XRD pattern, i.e., from comparison with fig. 1 (a), the relative intensity of the (104) diffraction peak is enhanced, and the orientation is enhanced. Mg synthesized by molten salt method in example 2 2 Zn 2 Ta 2 O 9 As is clear from the powder XRD pattern, i.e., from comparison with FIG. 1 (c), the relative intensity of the (104) diffraction peak is reduced, and the orientation is inferior to that of Mg 2 Zn 2 Ta 2 O 9 Is strong. The SEM photograph is shown in FIG. 5, from which it can be seen that Mg was synthesized by the molten salt method 4 TaNbO 9 Is sheet-shaped, has the radial length of 0.5 to 1.0 mu m and the thickness of 0.05 to 0.1 mu m, and has larger aspect ratio.
Example 4
(1) According to Mg 2 Zn 2 TaNbO 9 The reaction equation of (1) was calculated, and 4.0489g of MgO (99.99%), 8.1782g of ZnO (99.99%) and Ta were accurately weighed 2 O 5 (99.99％)11.0968g、Nb 2 O 5 (99.99%) 6.6761g, naCl (100%) 11.4738g, KCl (100%) 58.5262g, each with 50mL of absolute ethanol, grinding and mixing in agate mortar for 4h, transferring to a glass container, and oven drying. Sieving the dried raw material, and adding Al 2 O 3 And covering the crucible, and sintering in a muffle furnace at 950 ℃ for 1h at a heating and cooling rate of 100 ℃/h. Grinding the sintered sample to be crushed, transferring the crushed sintered sample to a glass cup, adding deionized water, heating the crushed sintered sample to 75 ℃ in a water bath, magnetically stirring the crushed sintered sample for 20min, performing suction filtration for 10 times to remove NaCl and KCl fused salt in the crushed sintered sample, and drying the crushed sintered sample at 80 ℃ for 8h to obtain a powder sample. FIG. 1 (e) shows Mg synthesized by the molten salt method 2 Zn 2 TaNbO 9 Powder XRD pattern, and Mg 4 Ta 2 O 9 The diffraction peaks of the PDF standard card (figure 1 (f)) #38-1458 are in one-to-one correspondence, and no impurity phase peak exists, which indicates that the powder synthesized by the molten salt method is a pure phase. Separately reacting with solid phase to synthesize Mg 4 Ta 2 O 9 Powder XRD pattern and fused salt method synthesized Mg 4 Ta 2 O 9 、Mg 2 Zn 2 Ta 2 O 9 、Mg 4 TaNbO 9 Comparing the powder XRD patterns, i.e., fig. 1 (a), (b), (c), and (d), respectively, it is found that (104) has the highest relative intensity of diffraction peak and the strongest orientation. The SEM photograph is shown in FIG. 6, from which it can be seen that Mg was synthesized by the molten salt method 2 Zn 2 TaNbO 9 Is sheet-shaped, has the radial length of 1-2 mu m and the thickness of 0.1-0.2 mu m, and has larger aspect ratio. There are also a large number of square particles with a particle size of 0.1 to 0.3 μm.
Claims (7)
1. SheetThe microcrystalline powder is characterized in that the chemical general formula of the microcrystalline powder is (Mg) x1- Zn x ) 4 (Ta y1- Nb y ) 2 O 9 Wherein x =0 to 1, y =0 to 1, the flaky microcrystalline powder has a grain orientation, and the SEM picture shows that the flaky microcrystalline powder is flaky and is formed by MgO, znO and Ta 2 O 5 、Nb 2 O 5 Is prepared by taking a precursor raw material and carrying out topological melting reaction in a NaCl-KCl molten salt system.
2. The flaky microcrystalline powder of claim 1, wherein the flaky microcrystalline powder has a radial length of 0.1 to 2.5 μm and a thickness of 0.05 to 0.3 μm.
3. The method for producing the flaky microcrystalline powder of claim 1 or 2, comprising: weighing precursor raw materials MgO, znO and Ta according to a chemical general formula and a stoichiometric ratio 2 O 5 And Nb 2 O 5 And weighing NaCl and KCl raw materials, grinding and uniformly mixing the raw materials with absolute ethyl alcohol, drying, sintering at 950 ℃ in a muffle furnace, grinding a sintered sample until the sintered sample is crushed, transferring the crushed sintered sample to a container, adding deionized water, removing NaCl and KCl fused salt by adopting a heating, stirring, dissolving and suction filtering method, and finally drying to obtain the flaky microcrystalline powder.
4. The method for preparing flaky microcrystalline powder according to claim 3, wherein the ratio of the sum of the masses of the raw materials NaCl and KCl to the sum of the masses of the raw materials of the precursors is 7:3.
5. the method for preparing flaky microcrystalline powder according to claim 4, wherein the molar ratio of NaCl to KCl is 4:6 or 2:8.
6. the method for preparing the flaky microcrystalline powder according to claim 3, wherein the temperature rise rate of the sintering is 80 to 120 ℃/h, and the time is 1 to 2h.
7. The use of the flaky microcrystalline powder of claim 1 or 2 in a microwave dielectric ceramic, a scintillating transparent ceramic or a glass microcrystalline scintillator.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4234436A (en) * | 1979-10-18 | 1980-11-18 | General Electric Company | Molten salt synthesis of modified alkali niobate powders |
| CN101805021A (en) * | 2009-02-17 | 2010-08-18 | 西北工业大学 | Preparation method of flaky sodium niobate microcrystalline powder |
| CN110342934A (en) * | 2019-06-19 | 2019-10-18 | 西安交通大学 | A kind of micron-stage sheet-like niobic acid sodium crystal and its preparation method and application |
| CN113372004A (en) * | 2021-07-01 | 2021-09-10 | 上海应用技术大学 | Borate scintillation microcrystalline glass and preparation method and application thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4234436A (en) * | 1979-10-18 | 1980-11-18 | General Electric Company | Molten salt synthesis of modified alkali niobate powders |
| CN101805021A (en) * | 2009-02-17 | 2010-08-18 | 西北工业大学 | Preparation method of flaky sodium niobate microcrystalline powder |
| CN110342934A (en) * | 2019-06-19 | 2019-10-18 | 西安交通大学 | A kind of micron-stage sheet-like niobic acid sodium crystal and its preparation method and application |
| CN113372004A (en) * | 2021-07-01 | 2021-09-10 | 上海应用技术大学 | Borate scintillation microcrystalline glass and preparation method and application thereof |
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