CN103570068B - A kind of niobite structure ZnNb 2o 6fiber and preparation method thereof - Google Patents

A kind of niobite structure ZnNb 2o 6fiber and preparation method thereof Download PDF

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CN103570068B
CN103570068B CN201310489069.0A CN201310489069A CN103570068B CN 103570068 B CN103570068 B CN 103570068B CN 201310489069 A CN201310489069 A CN 201310489069A CN 103570068 B CN103570068 B CN 103570068B
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koh
niobite
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孔新刚
郭章林
黄剑锋
欧阳海波
李翠艳
费杰
卢靖
曹丽云
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Shaanxi University of Science and Technology
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Abstract

The invention discloses a kind of niobite structure ZnNb 2o 6fiber and preparation method thereof, belongs to technical field of nanometer material preparation, and the inventive method is with Nb 2o 5be raw material with KOH, obtain the niobate presoma of solubility through hydrothermal treatment consists, subsequently the aqueous ethanolic solution of presoma and KOH is carried out solvent thermal reaction, prepare tunnel structure K 2nb 2o 6h 2o fiber, then with Zn (NO 3) 2for zinc source and tunnel type K 2nb 2o 6h 2k+ ion in O carries out ion exchange reaction, filters, washing, and dry, last thermal treatment, obtains niobite structure ZnNb 2o 6fiber.The niobite structure ZnNb that the present invention obtains 2o 6fiber by the nanocrystalline polycrystalline formed, and has orientation, and individual fiber diameter is about 1 ~ 5 μm, and length is 10 ~ 80 μm, and nanocrystalline granularity is 5 ~ 20nm.The invention provides the method preparing thread zinc niobate and have product good crystallinity, purity is high, and reaction conditions is gentle, simple to operate, the high and product morphology of repeatability and the advantage such as size is controlled.

Description

A kind of niobite structure ZnNb 2o 6fiber and preparation method thereof
Technical field
The invention belongs to technical field of nanometer material preparation, relate to a kind of niobite structure ZnNb 2o 6fiber and preparation method thereof.
Background technology
Zinc niobate has excellent optics, magnetics and dielectric properties, and be the critical material manufacturing wave filter resonator, zinc niobate also has extraordinary photocatalysis performance, especially in ultraviolet region response obviously, is that one of most active field studied by function ceramics in recent years.The performance of zinc niobate is relevant with microscopic appearance with its granularity, and both determine the performance of zinc niobate material to a great extent.Therefore, preparation has the focus that the nanometer particle of special appearance as thread, sheet etc. has become zinc niobate research.
At present, the preparation method of the nano level zinc niobate proposed both at home and abroad comprises solid-phase synthesis, sol-gel method, molten-salt growth method and solvent-thermal process method etc.No. 201210055058.7th, Chinese invention issued patents discloses a kind of liquid phase preparation process of zinc niobate microwave-medium ceramics, and the method is by Nb 2o 5after mixing with KOH, first melting, after add deionized water and dissolve, and adjust ph is to generating precipitation, obtains solubility niobium salt; Take solubility niobium salt and zinc sulfate, and add water and be made into mixing salt solution, then add dispersion agent, then add in reactor, with NaOH regulator solution pH, carry out coprecipitation reaction under certain condition; Gained throw out carried out wash, filter, dry, after grinding, pre-burning, adds binding agent and sintering agent, then sinters in the throw out then after pre-burning, obtains zinc niobate Microwave dielectric ceramic powder material.WeimingWu etc. are at WuW, LiangS, DingZ, etal.LowtemperaturesynthesisofnanosizedZnNb 2o 6adopt citric acid complex method in photocatlystsbyacitratecomplexmethod [Journalofsol-gelscienceandtechnology, 2012,61 (3): 570-576], obtain the ZnNb of size of particles at 50-150nm 2o 6.SangMinJi etc. are at SangMinJi, SunHeeChoi, etal, BandGapTailoredZn (Nb 1-xv x) 2o 6in SolidSolutionsasVisibleLightPhotocatalysts [Phys.Chem.C2009,113,17824 – 17830], high temperature solid-state method is utilized to synthesize the zinc niobate Zn (Nb of vanadium doping 1-xv x) 2o 6.
More than prepare the method for zinc niobate or need high-temperature calcination, or needing the additive such as binding agent and complexing agent, preparation condition requirement is high, step is numerous and diverse, efficiency is low, be unfavorable for suitability for industrialized production.
Summary of the invention
In order to overcome the defect that above-mentioned prior art exists, the object of the present invention is to provide a kind of niobite structure ZnNb 2o 6fiber and preparation method thereof, the method reaction conditions is gentle, without the need to additive, simple to operate, reproducible, by the niobite structure ZnNb that the method is obtained 2o 6fibre crystallinity is good, and purity is high.
The present invention is achieved through the following technical solutions:
A kind of niobite structure ZnNb 2o 6the preparation method of fiber, comprises the following steps:
1) according to the ratio of 1g:5 ~ 8ml, by Nb 2o 5joining concentration is in the KOH aqueous solution of 2 ~ 3mol/L, carries out hydrothermal treatment consists, obtains solubility niobate solution, in solubility niobate solution, add ethanol at 180 ~ 230 DEG C, separates out solubility niobate presoma;
2) according to the ratio of 1g:25 ~ 35ml, solubility niobate presoma is joined in the aqueous ethanolic solution of KOH, at 220 ~ 250 DEG C, carries out solvent thermal reaction, reacting liquid filtering must be precipitated, precipitate through washing, drying, obtain tunnel type structure K 2nb 2o 6fiber; Wherein, in the aqueous ethanolic solution of described KOH, the concentration of KOH is 0.5 ~ 1mol/L;
3) according to the ratio of 1g:80 ~ 120ml, by tunnel type structure K 2nb 2o 6fiber joins the Zn (NO that concentration is 0.5 ~ 1.5mol/L 3) 2in solution, filter after fully stirring, by washing of precipitate, drying, obtain tunnel type structure ZnNb 2o 6fiber;
4) by tunnel type structure ZnNb 2o 6fiber thermal treatment at 600 ~ 800 DEG C, obtains the ZnNb of niobite structure 2o 6fiber.
Ethanol described in step 1) is dehydrated alcohol, and and Nb 2o 5add according to the amount of 1g:5 ~ 8ml.
Hydrothermal conditions described in step 1) is 2 ~ 3h.
Step 2) described in KOH aqueous ethanolic solution in the volume ratio of second alcohol and water be 1 ~ 2:1.
Step 2) described in time of solvent thermal reaction be 9 ~ 14h.
Stirring described in step 3) at room temperature stirs 20 ~ 30h.
Heat treatment time described in step 4) is 2 ~ 3h.
Niobite structure ZnNb 2o 6fiber is the polycrystalline of nanocrystalline composition, and has orientation, and individual fiber diameter is 1 ~ 5 μm, and length is 10 ~ 80 μm, and nanocrystalline granularity is 5 ~ 20nm.
Compared with prior art, the present invention has following useful technique effect:
The present invention is with Nb 2o 5be raw material with KOH, obtain the niobate presoma of solubility through hydrothermal treatment consists, subsequently the aqueous ethanolic solution of presoma and KOH is carried out solvent thermal reaction, prepare tunnel structure K 2nb 2o 6h 2o fiber, then with Zn (NO 3) 2for zinc source and tunnel type K 2nb 2o 6h 2k in O +ion carries out ion exchange reaction, filters, washing, and dry, last thermal treatment, obtains niobite structure ZnNb 2o 6fiber.By control KOH and Zn (NO 3) 2concentration and thermal treatment temp can control pattern and the crystallinity of thread zinc niobate.The niobite structure ZnNb that the present invention obtains 2o 6fiber is by the nanocrystalline polycrystalline formed, and have orientation, individual fiber diameter is 1 ~ 4 μm, and length is 10 ~ 80 μm, nanocrystalline granularity is 5 ~ 20nm, good crystallinity, purity is high, and the present invention has reaction conditions gentleness, simple to operate, high and the product morphology of repeatability and the advantage such as size is controlled, environmental friendliness, is applicable to industrial amplification production.
Accompanying drawing explanation
Fig. 1 is the X-ray diffraction XRD figure spectrum of nanometer zinc niobate fiber prepared by the present invention;
Fig. 2 be the nanometer zinc niobate fiber prepared of the present invention scanning electron microscope sem photo;
Fig. 3 is the selected area electron diffraction point SAED photo of nanometer zinc niobate fiber prepared by the present invention, and wherein, (a) is transmission electron microscope photo, (b) selected area electron diffraction point photo.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, and the explanation of the invention is not limited.
Embodiment 1
A kind of niobite structure ZnNb 2o 6the preparation method of fiber, comprises the following steps:
1) 5.1gNb is got 2o 5join in the KOH aqueous solution of the 2mol/L of 30ml, at 200 DEG C, hydrothermal treatment consists 2h, obtains solubility niobate solution, is joined by 30ml dehydrated alcohol in this solution, precipitable go out solubility niobate presoma;
2) get the solubility niobate presoma of 1g, join in the aqueous ethanolic solution of 30mlKOH, at 230 DEG C, after solvent thermal reaction 12h, reacting liquid filtering must be precipitated, precipitate through washing, drying, obtain tunnel type structure K 2nb 2o 6fiber; Wherein, in described mixing solutions, the concentration of KOH is 0.5mol/L, and in the aqueous ethanolic solution of described KOH, the volume ratio of ethanol and water is 1:1;
3) configuration concentration is the Zn (NO of 0.5mol/L 3) 2solution, by tunnel type structure K 2nb 2o 6solution Zn (NO put into by fiber 3) 2in solution, stirred at ambient temperature 24h, makes Zn 2+by with K +ion-exchange enters into tunnel type structure, filters, and washing is dry, obtains tunnel type structure ZnNb 2o 6fiber; Tunnel type structure ZnNb will be obtained 2o 6fiber joins above-mentioned Zn (NO again 3) 2in solution, repeat to stir, filter, washing, drying step, makes Zn 2+with K +ion can fully exchange;
4) by tunnel type structure ZnNb 2o 6fiber thermal treatment at 600 DEG C, obtains the ZnNb of niobite structure 2o 6fiber.
What obtain through the present embodiment singlely forms ZnNb by nanocrystalline 2o 6the diameter of fiber is 1 μm, and length is 10 μm, and nanocrystalline granularity is 5nm.
See Fig. 1, be the ZnNb of obtained niobite structure 2o 6fiber XRD figure spectrum, by with niobite ZnNb 2o 6standard P DF card (37-1371) is compared, and proves that product prepared by the present invention is the ZnNb of niobite structure 2o 6.
See Fig. 2, be the ZnNb of obtained niobite structure 2o 6the SEM photo of fiber, can clearly find out from figure, niobite structure ZnNb 2o 6fibroplastic polycrystalline fibre.
See Fig. 3, (a) is transmission electron microscope photo, (b) selected area electron diffraction photo; Show hematite structure ZnNb 2o 6polycrystalline fibre is similar to single crystal diffraction spot, shows that it has orientation.Under normal conditions, the SAED photo of polycrystalline particle can demonstrate a diffraction and be similar to the single crystal diffraction spot ring of light, because the particle of composition polycrystalline is random alignment, and the particle forming polycrystalline is when aligning, and its SAED photo can demonstrate and be similar to single crystal diffraction spot.
Embodiment 2
A kind of niobite structure ZnNb 2o 6the preparation method of fiber, comprises the following steps:
1) 5.1gNb is got 2o 5join in the KOH aqueous solution of the 2mol/L of 30ml, at 180 DEG C, hydrothermal treatment consists 3h, obtains solubility niobate solution, is joined by 30ml dehydrated alcohol in this solution, precipitable go out solubility niobate presoma;
2) get the solubility niobate presoma of 1g, join in the aqueous ethanolic solution of 30mlKOH, at 230 DEG C, after solvent thermal reaction 12h, reacting liquid filtering must be precipitated, precipitate through washing, drying, obtain tunnel type structure K 2nb 2o 6fiber; Wherein, in described mixing solutions, the concentration of KOH is 1mol/L, and in the aqueous ethanolic solution of described KOH, the volume ratio of ethanol and water is 1:1;
3) configuration concentration is the Zn (NO of 1mol/L 3) 2solution, according to the ratio of 1g:120ml, by tunnel type structure K 2nb 2o 6solution Zn (NO put into by fiber 3) 2in solution, stirred at ambient temperature 20h, makes Zn 2+by with K +ion-exchange enters into tunnel type structure, filters, and washing is dry, obtains tunnel type structure ZnNb 2o 6fiber; Tunnel type structure ZnNb will be obtained 2o 6fiber joins above-mentioned Zn (NO again 3) 2in solution, repeat to stir, filter, washing, drying step, makes Zn 2+with K +ion can fully exchange;
4) by tunnel type structure ZnNb 2o 6fiber thermal treatment at 650 DEG C, obtains the ZnNb of niobite structure 2o 6fiber.
What obtain through the present embodiment singlely forms ZnNb by nanocrystalline 2o 6the diameter of fiber is 1 μm, and length is 10 μm, and nanocrystalline granularity is 7nm.
Embodiment 3
A kind of niobite structure ZnNb 2o 6the preparation method of fiber, comprises the following steps:
1) 5.0gNb is got 2o 5join in the KOH aqueous solution of the 3mol/L of 25ml, at 200 DEG C, hydrothermal treatment consists 3h, obtains solubility niobate solution, is joined by 25ml dehydrated alcohol in this solution, precipitable go out solubility niobate presoma;
2) the solubility niobate presoma getting 1g adds in the aqueous ethanolic solution of 25mlKOH, at 220 DEG C, after solvent thermal reaction 14h, must be precipitated by reacting liquid filtering, precipitates through washing, drying, obtains tunnel type structure K 2nb 2o 6fiber; Wherein, in described mixing solutions, the concentration of KOH is 1mol/L, and in the aqueous ethanolic solution of described KOH, the volume ratio of ethanol and water is 2:1;
3) configuration concentration is the Zn (NO of 1.5mol/L 3) 2solution, according to the ratio of 1g:80ml, by tunnel type structure K 2nb 2o 6solution Zn (NO put into by fiber 3) 2in solution, stirred at ambient temperature 24h, makes Zn 2+by with K +ion-exchange enters into tunnel type structure, filters, and washing is dry, obtains tunnel type structure ZnNb 2o 6fiber; Tunnel type structure ZnNb will be obtained 2o 6fiber joins above-mentioned Zn (NO again 3) 2in solution, repeat to stir, filter, washing, drying step, makes Zn 2+with K +ion can fully exchange;
4) by tunnel type structure ZnNb 2o 6fiber thermal treatment at 700 DEG C, obtains the ZnNb of niobite structure 2o 6fiber.
What obtain through the present embodiment singlely forms ZnNb by nanocrystalline 2o 6the diameter of fiber is 5 μm, and length is 80 μm, and nanocrystalline granularity is 12nm.
Embodiment 4
A kind of niobite structure ZnNb 2o 6the preparation method of fiber, comprises the following steps:
1) 5.0gNb is got 2o 5join in the KOH aqueous solution of the 3mol/L of 40ml, at 200 DEG C, hydrothermal treatment consists 3h, obtains solubility niobate solution, is joined by 40ml dehydrated alcohol in this solution, precipitable go out solubility niobate presoma;
2) the solubility niobate presoma getting 1g adds in the aqueous ethanolic solution of 35mlKOH, at 250 DEG C, after solvent thermal reaction 9h, must be precipitated by reacting liquid filtering, precipitates through washing, drying, obtains tunnel type structure K 2nb 2o 6fiber; Wherein, in described mixing solutions, the concentration of KOH is 1mol/L, and in the aqueous ethanolic solution of described KOH, the volume ratio of ethanol and water is 2:1;
3) configuration concentration is the Zn (NO of 1.5mol/L 3) 2solution, according to the ratio of 1g:100ml, by tunnel type structure K 2nb 2o 6solution Zn (NO put into by fiber 3) 2in solution, stirred at ambient temperature 30h, makes Zn 2+by with K +ion-exchange enters into tunnel type structure, filters, and washing is dry, obtains tunnel type structure ZnNb 2o 6fiber; Tunnel type structure ZnNb will be obtained 2o 6fiber joins above-mentioned Zn (NO again 3) 2in solution, repeat to stir, filter, washing, drying step, makes Zn 2+with K +ion can fully exchange;
4) by tunnel type structure ZnNb 2o 6fiber thermal treatment at 800 DEG C, obtains the ZnNb of niobite structure 2o 6fiber.
What obtain through the present embodiment singlely forms ZnNb by nanocrystalline 2o 6the diameter of fiber is 5 μm, and length is 80 μm, and nanocrystalline granularity is 20nm.

Claims (3)

1. a niobite structure ZnNb 2o 6the preparation method of fiber, is characterized in that, comprises the following steps:
1) according to the ratio of 1g:5 ~ 8ml, by Nb 2o 5joining concentration is in the KOH aqueous solution of 2 ~ 3mol/L, carries out hydrothermal treatment consists 2 ~ 3h, obtains solubility niobate solution, in solubility niobate solution, add ethanol at 180 ~ 230 DEG C, separates out solubility niobate presoma; Described ethanol is dehydrated alcohol, and and Nb 2o 5add according to the amount of 1g:5 ~ 8ml;
2) according to the ratio of 1g:25 ~ 35ml, solubility niobate presoma is joined in the aqueous ethanolic solution of KOH, at 220 ~ 250 DEG C, carries out solvent thermal reaction 9 ~ 14h, reacting liquid filtering must be precipitated, precipitate through washing, drying, obtain tunnel type structure K 2nb 2o 6fiber; Wherein, in the aqueous ethanolic solution of described KOH, the concentration of KOH is 0.5 ~ 1mol/L; In the aqueous ethanolic solution of described KOH, the volume ratio of second alcohol and water is 1 ~ 2:1;
3) according to the ratio of 1g:80 ~ 120ml, by tunnel type structure K 2nb 2o 6fiber joins the Zn (NO that concentration is 0.5 ~ 1.5mol/L 3) 2in solution, filter after fully stirring, by washing of precipitate, drying, obtain tunnel type structure ZnNb 2o 6fiber;
4) by tunnel type structure ZnNb 2o 6fiber is thermal treatment 2 ~ 3h at 600 ~ 800 DEG C, obtains the ZnNb of niobite structure 2o 6fiber.
2. a kind of niobite structure ZnNb according to claim 1 2o 6the preparation method of fiber, is characterized in that, step 3) described in stirring be at room temperature stir 20 ~ 30h.
3. the niobite structure ZnNb adopting the method in claim 1 ~ 2 described in any one obtained 2o 6fiber, is characterized in that, this niobite structure ZnNb 2o 6fiber is the polycrystalline of nanocrystalline composition, and has orientation, and individual fiber diameter is 1 ~ 5 μm, and length is 10 ~ 80 μm, and nanocrystalline granularity is 5 ~ 20nm.
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CN103936077B (en) * 2014-04-22 2015-09-02 江苏大学 A kind of preparation method of niobic acid manganese nano flower
CN106198867B (en) * 2016-07-04 2018-02-09 上海纳米技术及应用国家工程研究中心有限公司 A kind of ZnNb2O6The synthetic method of gas sensitive
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