CN103964505B - A kind of preparation method of columbite type metal niobate nanostructure - Google Patents
A kind of preparation method of columbite type metal niobate nanostructure Download PDFInfo
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 16
- 239000002184 metal Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 16
- 150000003839 salts Chemical class 0.000 claims abstract description 6
- 239000002243 precursor Substances 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 23
- 239000000243 solution Substances 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- 229910052759 nickel Inorganic materials 0.000 claims description 11
- 239000000047 product Substances 0.000 claims description 9
- 239000007795 chemical reaction product Substances 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 6
- 238000012546 transfer Methods 0.000 claims description 6
- 239000011575 calcium Chemical class 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 5
- 230000008020 evaporation Effects 0.000 claims description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical class [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 4
- 229910052791 calcium Inorganic materials 0.000 claims description 4
- 229910017052 cobalt Inorganic materials 0.000 claims description 4
- 239000010941 cobalt Substances 0.000 claims description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical class [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 229910052788 barium Inorganic materials 0.000 claims description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical class [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052793 cadmium Inorganic materials 0.000 claims description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 229910052712 strontium Inorganic materials 0.000 claims description 2
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical class [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 2
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims 2
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims 1
- 238000001816 cooling Methods 0.000 claims 1
- 229910052742 iron Inorganic materials 0.000 claims 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical class [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims 1
- 239000011259 mixed solution Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- BDRTVPCFKSUHCJ-UHFFFAOYSA-N molecular hydrogen;potassium Chemical compound [K].[H][H] BDRTVPCFKSUHCJ-UHFFFAOYSA-N 0.000 claims 1
- 238000003756 stirring Methods 0.000 claims 1
- 229910052725 zinc Inorganic materials 0.000 claims 1
- 239000011701 zinc Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 19
- -1 niobium potassium hydrogen phthalate Chemical compound 0.000 abstract description 14
- 239000010955 niobium Substances 0.000 abstract description 10
- 238000002156 mixing Methods 0.000 abstract description 9
- 229910052758 niobium Inorganic materials 0.000 abstract description 9
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 abstract description 9
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000007791 liquid phase Substances 0.000 abstract description 2
- 238000001953 recrystallisation Methods 0.000 abstract description 2
- 239000012153 distilled water Substances 0.000 description 15
- 239000002253 acid Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 10
- 239000000725 suspension Substances 0.000 description 10
- 238000001914 filtration Methods 0.000 description 6
- 238000002844 melting Methods 0.000 description 6
- 230000008018 melting Effects 0.000 description 6
- 206010013786 Dry skin Diseases 0.000 description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 230000001186 cumulative effect Effects 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 5
- 238000003760 magnetic stirring Methods 0.000 description 5
- 239000011591 potassium Substances 0.000 description 5
- 229910052700 potassium Inorganic materials 0.000 description 5
- 238000000967 suction filtration Methods 0.000 description 5
- 238000000137 annealing Methods 0.000 description 4
- 239000011572 manganese Substances 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 3
- 229910052748 manganese Inorganic materials 0.000 description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 150000001342 alkaline earth metals Chemical class 0.000 description 2
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- RPEUFVJJAJYJSS-UHFFFAOYSA-N zinc;oxido(dioxo)niobium Chemical compound [Zn+2].[O-][Nb](=O)=O.[O-][Nb](=O)=O RPEUFVJJAJYJSS-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229910021380 Manganese Chloride Inorganic materials 0.000 description 1
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 description 1
- 229910005805 NiNb Inorganic materials 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- DBJUEJCZPKMDPA-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O DBJUEJCZPKMDPA-UHFFFAOYSA-N 0.000 description 1
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000005290 antiferromagnetic effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
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- 230000005611 electricity Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000005291 magnetic effect Effects 0.000 description 1
- 239000011565 manganese chloride Substances 0.000 description 1
- 235000002867 manganese chloride Nutrition 0.000 description 1
- 229940099607 manganese chloride Drugs 0.000 description 1
- CNFDGXZLMLFIJV-UHFFFAOYSA-L manganese(II) chloride tetrahydrate Chemical compound O.O.O.O.[Cl-].[Cl-].[Mn+2] CNFDGXZLMLFIJV-UHFFFAOYSA-L 0.000 description 1
- 238000010303 mechanochemical reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
A kind of preparation method of columbite shaped metal niobate nanostructure, after it is characterized in that first utilizing Niobium Pentxoxide and molten potassium hydroxide reaction, recrystallization prepares six niobium potassium hydrogen phthalate forerunners in aqueous, re-use six niobium potassium hydrogen phthalates and soluble metallic salt carries out hydro-thermal reaction, form metal niobates finally by carrying out washing treatment.Technological method involved in the present invention has following obvious advantage: 1. the present invention uses hydrothermal technique, and technique is simple, and easy to operate, production cost is low, and environmentally friendly; 2. this synthetic technology can be carried out under lower temperature of reaction; 3. whole reaction carries out in the liquid phase, and the mixing of precursor is full and uniform; 4. the preparation of the method to metal niobates series has obvious universality.
Description
Technical field
The invention belongs to inorganic material chemistry field, relate to a kind of preparation method of columbite niobate.
Background technology
Columbite structural metal niobate ceramics material generally can be expressed as ANb
2o
6type general. formula, wherein A is divalent alkaline-earth metal or transition metal.First, this kind of material has higher specific inductivity and lower dissipation loss at microwave frequencies, therefore can have huge applications potentiality in satellite communication field as dielectric resonator material; Secondly, the columbite niobate that part comprises magnetic ion can show unique antiferromagnetic character; Finally, this series material also has the character such as excellent electricity, electrochemistry, optics and catalysis.
At present, preparing the topmost method of columbite niobate is solid-phase synthesis, and namely utilize Niobium Pentxoxide and metal simple-substance, oxide compound or carbonate to be raw material, at high temperature (>=1000 DEG C) carry out calcining and obtaining.These class methods require heating for multiple times and grinding usually, and need atmosphere protection, and gained sample generally has larger size, and do not have well-regulated form.Therefore, the method complex process equipment, energy consumption is comparatively large, and production cost is high.In recent years, other chemical preparation process are also constantly applied to the preparation of columbite niobate, as: mechanochemical reaction, sol-gel method, coprecipitation method etc., but these methods be substantially for precursor homogeneous phase mixing and design, obtain final columbite niobate product, still need further high-temperature process.Therefore, explore a kind of simple, pervasive preparation method to synthesize columbite type niobate series compound, especially prepare its nanostructure, there is larger challenge and important Research Significance all the time.
Summary of the invention
In order to overcome making excessive demands to hot conditions in niobate prior synthesizing method, the present invention proposes a kind of universality method preparing columbite shaped metal niobate nanostructure under cryogenic.The method is without the need to complex apparatus, and processing condition are simple, and easy handling controls, and synthesis cost is low.
The present invention is achieved by the following technical solutions.
1) preparation of six niobium potassium hydrogen phthalate presomas.Potassium hydroxide (KOH) is placed in nickel crucible heating and melting, then adds Niobium Pentxoxide (Nb
2o
5), the mass ratio of potassium hydroxide and Niobium Pentxoxide is 3 ~ 7:1, after question response is complete, naturally cool to room temperature, soluble in water for gained material, filter and remove not molten thing, obtained soln using heating evaporation or subcooled method are carried out recrystallization, wash with the mixing solutions of ethanol and water again after filtration, after drying, can presoma be obtained.
2) hydro-thermal reaction.Stoichiometrically take six niobium potassium hydrogen phthalate presomas prepared in soluble metallic salt and step 1), water-soluble respectively, then two kinds of aqueous solution are under agitation mixed, be then transferred in hydrothermal reaction kettle, 150 ~ 200 DEG C of constant temperature sealed reactions, are cooled to room temperature after reaction terminates.
3) carrying out washing treatment.By step 2) in hydro-thermal reaction product filter, with the alternately washing of water and ethanol, remove the ion that unreacted is complete, obtained columbite metal niobates product after dry.
Step 2 of the present invention) described in soluble metallic salt be one in the divalent alkaline-earth metal of magnesium (Mg), calcium (Ca), strontium (Sr), barium (Ba), manganese (Mn), iron (Fe), cobalt (Co), nickel (Ni), zinc (Zn), cadmium (Cd), copper (Cu) etc. or transition metal.
Metal niobates prepared by the present invention has typical orthorhombic phase columbite structure, and product is made up of nano particle or the multilevel hierarchy with nano particle by primitive.
Technological method involved in the present invention has following obvious advantage: 1. the present invention uses hydrothermal technique, and technique is simple, and easy to operate, production cost is low, and environmentally friendly; 2. this synthetic technology can be carried out under lower temperature of reaction; 3. whole reaction carries out in the liquid phase, and the mixing of precursor is full and uniform; 4. the preparation of the method to metal niobates series has obvious universality.
Accompanying drawing explanation
Fig. 1 is the X-ray diffracting spectrum of embodiment 1 sample.
Fig. 2 is the electron scanning micrograph of embodiment 1 sample.
Fig. 3 is the X-ray diffracting spectrum of embodiment 2 sample after 800 DEG C of annealing.
Fig. 4 is the electron scanning micrograph of embodiment 2 sample after 800 DEG C of annealing.
Fig. 5 is the X-ray diffracting spectrum of embodiment 3 sample after 800 DEG C of annealing.
Fig. 6 is the electron scanning micrograph of embodiment 3 sample after 800 DEG C of annealing.
Fig. 7 is the X-ray diffracting spectrum of embodiment 4 sample.
Fig. 8 is the electron scanning micrograph of embodiment 4 sample.
Embodiment
In order to understand the present invention better, below in conjunction with specific embodiment, the present invention will be further described, but protection content of the present invention is not limited to the following example.
Embodiment 1: niobic acid manganese (MnNb
2o
6) preparation.
1) 10g potassium hydroxide is placed in nickel crucible heating and melting, then 2g Niobium Pentxoxide is slowly added, room temperature is cooled to after reacting completely, gained material is dissolved in 150mL distilled water, filter and remove not molten thing, heating evaporation at gained settled solution 90 DEG C is obtained needle-like crystal, washs with the mixing solutions of ethanol and water (volume ratio is 1:1) after filtering, after drying, obtain six niobium potassium hydrogen phthalate presomas.
2) take 0.6mmol Manganous chloride tetrahydrate, 0.2mmol six niobium potassium hydrogen phthalate presoma, is dissolved in 10mL distilled water respectively.Under magnetic stirring, manganese chloride solution is added drop-wise to gradually in six niobic acid hydrogen potassium solutions, forms suspension.
3) by gained suspension transfer hydrothermal reaction kettle, add distilled water to about 80% of cumulative volume, sealing, 150 DEG C of isothermal reactions 12 ~ 24 hours, after reaction terminates, naturally cool to room temperature.
4) hydro-thermal reaction product is carried out suction filtration, alternately wash for several times with water and ethanol, 50 DEG C of dryings 6 hours, obtain niobic acid manganese powdered product.
Embodiment 2: niobic acid cobalt (CoNb
2o
6) preparation.
1) 10g potassium hydroxide is placed in nickel crucible heating and melting, then 2g Niobium Pentxoxide is slowly added, room temperature is cooled to after reacting completely, gained material is dissolved in 150mL distilled water, filter and remove not molten thing, heating evaporation at gained settled solution 90 DEG C is obtained needle-like crystal, washs with the mixing solutions of ethanol and water (volume ratio is 1:1) after filtering, after drying, obtain six niobium potassium hydrogen phthalate presomas.
2) take 0.6mmol cobalt chloride, 0.2mmol six niobium potassium hydrogen phthalate presoma, is dissolved in 10mL distilled water respectively.Under magnetic stirring, cobalt chloride solution is added drop-wise to gradually in six niobic acid hydrogen potassium solutions, forms suspension.
3) by gained suspension transfer hydrothermal reaction kettle, add distilled water to about 80% of cumulative volume, sealing, 180 DEG C of isothermal reactions 12 hours, after reaction terminates, naturally cool to room temperature.
4) hydro-thermal reaction product is carried out suction filtration, alternately wash for several times with water and ethanol, 50 DEG C of dryings 6 hours, obtain niobic acid cobalt dust product.
Embodiment 3: niobic acid nickel (NiNb
2o
6) preparation.
1) 10g potassium hydroxide is placed in nickel crucible heating and melting, then 2g Niobium Pentxoxide is slowly added, room temperature is cooled to after reacting completely, gained material is dissolved in 150mL distilled water, filter and remove not molten thing, heating evaporation at gained settled solution 90 DEG C is obtained needle-like crystal, washs with the mixing solutions of ethanol and water (volume ratio is 1:1) after filtering, after drying, obtain six niobium potassium hydrogen phthalate presomas.
2) take 0.6mmol nickelous chloride, 0.2mmol six niobium potassium hydrogen phthalate presoma, is dissolved in 10mL distilled water respectively.Under magnetic stirring, nickel chloride solution is added drop-wise to gradually in six niobic acid hydrogen potassium solutions, forms suspension.
3) by gained suspension transfer hydrothermal reaction kettle, add distilled water to about 80% of cumulative volume, sealing, 180 DEG C of isothermal reactions 12 hours, after reaction terminates, naturally cool to room temperature.
4) hydro-thermal reaction product is carried out suction filtration, alternately wash for several times with water and ethanol, 50 DEG C of dryings 6 hours, obtain niobic acid nickel by powder product.
Embodiment 4: calcium niobate (CaNb
2o
6) preparation.
1) 10g potassium hydroxide is placed in nickel crucible heating and melting, then 2g Niobium Pentxoxide is slowly added, room temperature is cooled to after reacting completely, gained material is dissolved in 150mL distilled water, filter and remove not molten thing, the refrigerator and cooled that gained settled solution is placed in 2 ~ 3 DEG C is but obtained needle-like crystal, washs with the mixing solutions of ethanol and water (volume ratio is 1:1) after filtering, after drying, obtain six niobium potassium hydrogen phthalate presomas.
2) take 0.6mmol calcium chloride, 0.2mmol six niobium potassium hydrogen phthalate presoma, is dissolved in 10mL distilled water respectively.Under magnetic stirring, calcium chloride solution is added drop-wise to gradually in six niobic acid hydrogen potassium solutions, forms suspension.
3) by gained suspension transfer hydrothermal reaction kettle, add distilled water to about 80% of cumulative volume, sealing, 160 DEG C of isothermal reactions 12 hours, after reaction terminates, naturally cool to room temperature.
4) hydro-thermal reaction product is carried out suction filtration, alternately wash for several times with water and ethanol, 50 DEG C of dryings 6 hours, obtain calcium niobate powdered product.
Embodiment 5: zinc niobate (ZnNb
2o
6) preparation.
1) 10g potassium hydroxide is placed in nickel crucible heating and melting, then 2g Niobium Pentxoxide is slowly added, room temperature is cooled to after reacting completely, gained material is dissolved in 150mL distilled water, filter and remove not molten thing, the refrigerator and cooled that gained settled solution is placed in 2 ~ 3 DEG C is but obtained needle-like crystal, washs with the mixing solutions of ethanol and water (volume ratio is 1:1) after filtering, after drying, obtain six niobium potassium hydrogen phthalate presomas.
2) take 0.6mmol zinc acetate, 0.2mmol six niobium potassium hydrogen phthalate presoma, is dissolved in 10mL distilled water respectively.Under magnetic stirring, acetic acid zinc solution is added drop-wise to gradually in six niobic acid hydrogen potassium solutions, forms suspension.
3) by gained suspension transfer hydrothermal reaction kettle, add distilled water to about 80% of cumulative volume, sealing, 180 DEG C of isothermal reactions 12 hours, after reaction terminates, naturally cool to room temperature.
4) hydro-thermal reaction product is carried out suction filtration, alternately wash for several times with water and ethanol, 50 DEG C of dryings 6 hours, obtain zinc niobate powdered product.
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| CN105712403A (en) * | 2016-04-15 | 2016-06-29 | 合肥国轩高科动力能源有限公司 | Preparation method of nano niobium pentoxide powder for lithium ion battery cathode material |
| CN106395903A (en) * | 2016-08-31 | 2017-02-15 | 周口师范学院 | Method for synthesis of hexaniobate and alkali metal salt using household microwave oven |
| CN109273280B (en) * | 2018-08-06 | 2020-02-21 | 江苏大学 | A kind of flexible composite electrode material, preparation method and application thereof |
| CN113582715A (en) * | 2020-12-30 | 2021-11-02 | 苏州金宏气体股份有限公司 | Nickel doped KNbO3Piezoelectric ceramic, preparation method thereof and high-purity hydrogen production |
| CN113042033B (en) * | 2021-01-20 | 2022-07-22 | 西南交通大学 | A method and material application for improving crystallization degree of columbine phase multi-element oxide material |
| CN113401943B (en) * | 2021-06-16 | 2022-05-10 | 福州大学 | Transition-rare earth dissimilar metal cluster doped multi-niobium oxyacid compound and preparation method thereof |
| CN114551892B (en) * | 2022-04-27 | 2022-08-02 | 浙江清华柔性电子技术研究院 | Cobalt niobate oxide-loaded graphene composite material and preparation method and application thereof |
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