CN115924970A - Potassium niobate nanowire and preparation method thereof - Google Patents
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- CN115924970A CN115924970A CN202211138317.2A CN202211138317A CN115924970A CN 115924970 A CN115924970 A CN 115924970A CN 202211138317 A CN202211138317 A CN 202211138317A CN 115924970 A CN115924970 A CN 115924970A
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- 239000002070 nanowire Substances 0.000 title claims abstract description 67
- UKDIAJWKFXFVFG-UHFFFAOYSA-N potassium;oxido(dioxo)niobium Chemical compound [K+].[O-][Nb](=O)=O UKDIAJWKFXFVFG-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title abstract description 9
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 111
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 32
- 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 abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 12
- 238000011049 filling Methods 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 238000007789 sealing Methods 0.000 claims abstract description 9
- 238000005303 weighing Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract 2
- 239000008367 deionised water Substances 0.000 claims description 21
- 229910021641 deionized water Inorganic materials 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000012528 membrane Substances 0.000 claims description 5
- 239000011148 porous material Substances 0.000 claims description 4
- 238000001471 micro-filtration Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 7
- 238000010438 heat treatment Methods 0.000 abstract description 6
- 230000003287 optical effect Effects 0.000 abstract description 6
- 238000003860 storage Methods 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 description 15
- 238000001027 hydrothermal synthesis Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 239000001103 potassium chloride Substances 0.000 description 2
- 235000011164 potassium chloride Nutrition 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000012374 esterification agent Substances 0.000 description 1
- 239000007863 gel particle Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000012982 microporous membrane Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention relates to the technical field of material science, in particular to a potassium niobate superfine nanowire with good crystallinity and a preparation method thereof. The flexible potassium niobate nanowire is characterized in that the diameter of the nanowire is 5-30nm, and the ratio of the length to the diameter of the nanowire is more than 50. The method comprises the following steps: step 1: weighing niobium pentoxide and potassium hydroxide, adding water, and uniformly mixing to ensure that the concentration of the potassium hydroxide is 5-8.5 mol/L; step 2: adding the mixed solution prepared in the step 1 into a reaction kettle, wherein the volume filling amount is 85-95%, sealing, heating to 180-240 ℃ by a program, preserving heat for 8-16 hours, and cooling; filtering, washing and drying. The potassium niobate nanowire prepared by the method has good crystallinity, the diameter of only about 5 to 20 nanometers, the length of several micrometers, high purity and the length-diameter ratio of more than 50, and can be widely applied to the fields of optical waveguide, frequency doubling, holographic storage and the like.
Description
Technical Field
The invention relates to the technical field of material science, in particular to a potassium niobate superfine nanowire with good crystallinity and a preparation method thereof.
Background
KNbO 3 The nano material is an important environment-friendly nano material with a perovskite structure, has excellent nonlinear optical characteristics, photocatalytic properties, electrocatalytic properties and the like, and is widely applied to optical waveguides and secondaryHarmonic, holographic storage, etc. Compared with other nanometer material structures, the one-dimensional nanometer line can show unique mechanical, optical and electrical properties on the nanometer scale. KNbO 3 The nano-wire can be used as a basic structural unit of a nano device, is designed and assembled into nano devices such as a nano generator, a nano laser, a gas sensor and the like at present, and has a very wide application prospect.
Preparation of KNbO 3 The methods of the nanowire include a hydrothermal method, a template method, a molten salt method, a precursor method and the like. The molten salt method is to mix and calcine potassium chloride and niobium pentoxide to synthesize KNb 3 O 8 Nanowires treated with nitric acid to give H 3 ONb 3 O 8 Nanowire, nb after calcination 2 O 5 Templating the nanowire and then adding Nb 2 O 5 Hydrothermal reaction of nano wire with KOH, KCl and the like to obtain KNbO 3 The nano-wire is complex in method, low in efficiency and high in cost. The template method generally comprises the steps of pouring sol-gel particles into pores such as alumina and the like, and reacting to synthesize KNbO 3 Then, the alumina template is etched off, and the KNbO synthesized by the method 3 Generally, the material is a polycrystalline material, the crystallinity is poor, an alumina template cannot be recycled, the cost is high, and the synthesis efficiency is low. The precursor method is generally to synthesize KNbO by a polymer precursor method by using coordination compounds, esterification agents and the like to be matched with metal ions 3 The shape of the product of the method is difficult to control, and the synthesis method is complex. The currently reported hydrothermal method takes potassium hydroxide and niobium pentoxide powder as raw materials, requires seven days of reaction time, is long in time, low in synthesis efficiency and poor in repeatability.
Besides the determination of low synthesis efficiency, poor repeatability and the like, the KNbO synthesized at present 3 The length-diameter ratio of the nanowire is low, and the diameter of the nanowire is more than 50 nm. The nanowires with large diameter and low length-diameter ratio have small specific surface area, and have poor electrical conductivity, thermal conductivity, optical performance and chemical stability. Therefore, KNbO with high length-diameter ratio and thin diameter is developed 3 The nano-wire has great economic benefit and social benefit.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a potassium niobate nanowire with good crystallinity and a preparation method thereof, wherein the diameter of the nanowire is only about 5 to 20 nanometers, the length of the nanowire is several micrometers, the purity is high, and the length-diameter ratio is more than 50; the preparation method of the nanowire takes potassium hydroxide and niobium pentoxide as raw materials, and the raw materials are directly mixed and then subjected to hydrothermal reaction, so that the method is simple, short in reaction time, good in repeatability, high in yield and low in cost.
In order to realize the purpose of the invention, the invention is realized by the following technical scheme:
the potassium niobate nanowire has the diameter of 5 to 30nm, the ratio of the length to the diameter of the nanowire is larger than 50, and the nanowire can be bent and has certain flexibility.
Preferably, the diameter of the nanowire is 5 to 20 nm
The potassium niobate (KNbO) is 3 ) The preparation method of the superfine nanowire comprises the following steps:
step 1: weighing niobium pentoxide and potassium hydroxide, putting the niobium pentoxide and the potassium hydroxide into a beaker, adding deionized water to ensure that the concentration of the potassium hydroxide is 5-8.5 mol/L, and stirring the materials by magnetic force to fully mix the materials uniformly to obtain a mixed solution;
step 2: adding the mixed solution into a high-pressure reaction kettle, sealing, putting into an oven, heating to 180-240 ℃, preserving heat for 8-16 hours, and cooling along with the oven, wherein the volume filling amount is 85-95%; filtering, washing and drying.
Further, the molar ratio of the potassium hydroxide to the niobium pentoxide in the step 1 is (85-100): 1.
Further, the temperature programming speed in the step 2 is 1 to 20 ℃/min; preferably 1 to 5 ℃/min.
Further, the filtration step described in step 2 uses a microfiltration membrane, wherein the pore size of the microfiltration membrane is 0.05-0.5um, preferably 0.1um.
Further, the washing step described in step 2 comprises washing several times with deionized water and absolute ethanol.
Further, the drying temperature in the step 2 is 45 to 100 ℃.
Compared with the prior art, the invention has the following beneficial effects:
firstly, the preparation method of the superfine potassium niobate nanowire provided by the invention has the advantages of simple raw materials, simple operation method, short reaction time, good repeatability, high yield and low cost. Secondly, the potassium niobate nanowire prepared by the method has good crystallinity, the diameter of only about 5 to 20 nanometers, the length of several micrometers, high purity and the length-diameter ratio of more than 50, and can be widely applied to the fields of optical waveguide, frequency doubling, holographic storage and the like.
Drawings
Fig. 1 is an SEM photograph of potassium niobate nanowires prepared in example 1.
FIG. 2 TEM photograph of potassium niobate nanowires prepared in example 1.
FIG. 3 shows the polycrystalline diffraction spectrum of the potassium niobate nanowire prepared in example 1.
FIG. 4 TEM photograph of potassium niobate nanowires prepared in example 2.
FIG. 5 is XRD spectrum of potassium niobate nanowire prepared in example 2.
Figure 6 TEM photograph of potassium niobate nanowires prepared in example 3.
FIG. 7 XRD spectrum of potassium niobate nanowire prepared in example 3.
Figure 8 is the polycrystalline diffraction pattern of potassium niobate nanowires prepared in example 3.
Fig. 9 TEM photograph of potassium niobate nanowires prepared in comparative example 1.
Fig. 10 TEM photograph of potassium niobate nanowire prepared in comparative example 2.
Fig. 11 TEM photograph of potassium niobate nanowires prepared in comparative example 3.
Detailed Description
The present application is described in further detail below by way of examples to enable those skilled in the art to practice the present application. It is to be understood that other embodiments may be utilized and that changes may be made without departing from the spirit or scope of the present application. To avoid detail not necessary to enable those skilled in the art to practice the application, the description may omit certain information known to those skilled in the art. The following detailed description is, therefore, not to be taken in a limiting sense, and the scope of the present invention is defined only by the appended claims. The following examples are presented to facilitate a better understanding of the present application and are not intended to limit the scope of the present application.
Example 1
Weighing niobium pentoxide and potassium hydroxide, putting the niobium pentoxide and the potassium hydroxide into a plastic beaker, and adding 90ml of deionized water to ensure that the concentration of the potassium hydroxide is 5mol/L and the addition amount of the niobium pentoxide is 0.005mol; magnetic stirring, adding the uniformly mixed solution into a 100ml high-pressure reaction kettle, wherein the volume filling amount is 90%, sealing, putting into an oven, heating to 180 ℃ at a heating rate of 3 ℃ per minute, keeping the temperature for 12 hours, and cooling along with the oven; taking out the reaction autoclave, guiding out the product, using a suction filter to suction-filter the product liquid with a microporous filter membrane (the aperture is 0.1 um), washing the product liquid with deionized water and absolute ethyl alcohol for a plurality of times, and putting the washed product into an oven to be dried at 60 ℃.
The SEM photograph of the obtained product is shown in figure 1, and it can be seen from the figure that the prepared potassium niobate nanowire can be bent and has certain flexibility; the TEM photograph is shown in fig. 2, it can be seen that the potassium niobate nanowire is less in aggregation degree, the diameter of the nanowire is about 10 nm, the length is about several microns, and the aspect ratio is higher than 100; the polycrystalline diffraction spectrum of the obtained product is shown in figure 3, and the potassium niobate nanowire prepared by the method has good crystallinity and high purity.
Example 2
Weighing niobium pentoxide and potassium hydroxide, putting the niobium pentoxide and the potassium hydroxide into a plastic beaker, and adding 85ml of deionized water to ensure that the concentration of the potassium hydroxide is 7mol/L and the addition amount of the niobium pentoxide is 0.007mol; and (4) stirring by magnetic force to fully and uniformly mix the components. The uniformly mixed solution of niobium pentoxide, potassium hydroxide and deionized water was added to a 100ml autoclave at a volume fill of 85%. After sealing, putting the mixture into an oven, heating to 200 ℃ at a heating rate of 5 ℃ per minute, preserving heat for 10 hours, and cooling along with the oven; the reaction autoclave was taken out, the product liquid was suction-filtered with a microporous membrane (pore diameter 0.1 um) using a suction filter, and washed several times with deionized water and anhydrous ethanol. And putting the cleaned product into an oven to be dried at 60 ℃.
The TEM photograph of the obtained product is shown in fig. 4, which shows that the potassium niobate nanowire has a relatively small agglomeration degree, a nanowire diameter of about 20 nm, a length of about several microns, a length-diameter ratio higher than 100, can be bent, and has a certain flexibility; the XRD spectrogram of the obtained product is shown in figure 5, and the prepared potassium niobate nanowire has good crystallinity and high purity.
Example 3
Weighing niobium pentoxide and potassium hydroxide, putting the niobium pentoxide and the potassium hydroxide into a plastic beaker, and adding 90ml of deionized water to ensure that the concentration of the potassium hydroxide is 8.5mol/L and the addition amount of the niobium pentoxide is 0.008mol; and (4) stirring by magnetic force to fully and uniformly mix. Adding a uniformly mixed solution of niobium pentoxide, potassium hydroxide and deionized water into a 100ml high-pressure reaction kettle, wherein the volume filling amount is 90%; after sealing, putting the mixture into an oven, raising the temperature to 200 ℃ at a temperature rise rate of 2 ℃ per minute, preserving the heat for 8 hours, and cooling the mixture along with the oven; taking out the reaction autoclave, guiding out the product, using a suction filter to suction-filter the product liquid by a microporous filter membrane (with the aperture of 0.1 um), and washing the product liquid by deionized water and absolute ethyl alcohol for a plurality of times; and putting the cleaned product into an oven to be dried at 100 ℃.
The TEM photograph of the obtained product is shown in fig. 6, which shows that the potassium niobate nanowire is less in agglomeration degree, the diameter of the nanowire is about 20 nm, the length of the nanowire is about several microns, the length-diameter ratio is higher than 100, and the potassium niobate nanowire can be bent and has certain flexibility. The XRD spectrogram and the polycrystalline diffractogram of the obtained product are shown in figures 7 and 8 respectively, and the fact that the synthesized potassium niobate nanowire is good in crystallinity and high in purity can be seen.
Comparative example 1
Weighing niobium pentoxide and potassium hydroxide, putting the niobium pentoxide and the potassium hydroxide into a plastic beaker, and adding 90ml of deionized water to ensure that the concentration of the potassium hydroxide is 15mol/L and the addition amount of the niobium pentoxide is 0.005mol; and (4) stirring by magnetic force to fully and uniformly mix the components. Adding a uniformly mixed solution of niobium pentoxide, potassium hydroxide and deionized water into a 100ml high-pressure reaction kettle, wherein the volume filling amount is 90%; after sealing, putting the mixture into an oven, raising the temperature to 200 ℃ at a temperature rise rate of 5 ℃ per minute, preserving the heat for 12 hours, and cooling the mixture along with the oven; taking out the reaction autoclave, taking out the product, and washing with deionized water and absolute ethyl alcohol for a plurality of times; and putting the cleaned product into an oven to be dried at 100 ℃.
The TEM photograph of the resulting product is shown in fig. 9, and it can be seen that potassium niobate nanowires tend to be formed, but the nanowires have a rough surface, indicating poor crystallinity, and have a diameter of about 500 nm and an aspect ratio of less than 5. The concentration of the potassium hydroxide in the method is as high as 15mol/L, and the prepared nano wire has lower length-diameter ratio and poor crystallinity.
Comparative example 2
Weighing niobium pentoxide and potassium hydroxide, putting the niobium pentoxide and the potassium hydroxide into a plastic beaker, and adding 90ml of deionized water to ensure that the concentration of the potassium hydroxide is 8.0mol/L and the addition amount of the niobium pentoxide is 0.005mol; and (4) stirring by magnetic force to fully and uniformly mix the components. Adding a uniformly mixed solution of niobium pentoxide, potassium hydroxide and deionized water into a 100ml high-pressure reaction kettle, wherein the volume filling amount is 90%; after sealing, putting the mixture into an oven, raising the temperature to 200 ℃ at a temperature rise rate of 5 ℃ per minute, preserving the heat for 72 hours, and cooling the mixture along with the oven; taking out the reaction autoclave, taking out the product, and washing with deionized water and absolute ethyl alcohol for a plurality of times; and putting the cleaned product into an oven to be dried at 100 ℃.
The TEM photograph of the obtained product is shown in fig. 10, and it can be seen that the diameter of the potassium niobate nanowire is about 50nm, and the aspect ratio is only about 10. The reaction time of the method is as long as 72h, and the length-diameter ratio of the prepared nanowire is low.
Comparative example 3
Weighing niobium pentoxide and potassium hydroxide, putting the niobium pentoxide and the potassium hydroxide into a plastic beaker, and adding 70ml of deionized water to ensure that the concentration of the potassium hydroxide is 8.0mol/L and the addition amount of the niobium pentoxide is 0.005mol; and (4) stirring by magnetic force to fully and uniformly mix the components. Adding a uniformly mixed solution of niobium pentoxide, potassium hydroxide and deionized water into a 100ml high-pressure reaction kettle, wherein the volume filling amount is 70%; after sealing, putting the mixture into an oven, raising the temperature to 200 ℃ at a temperature rise rate of 5 ℃ per minute, preserving the heat for 12 hours, and cooling the mixture along with the oven; taking out the reaction autoclave, taking out the product, and washing with deionized water and absolute ethyl alcohol for several times; and putting the cleaned product into an oven to be dried at 100 ℃.
The TEM photograph of the obtained product is shown in fig. 11, and it can be seen that the potassium niobate is square or irregular and is not a one-dimensional nanomaterial. Indicating that the potassium niobate nanowires can not be obtained by the hydrothermal reaction at low filling degree.
The contrast comparison example shows that the single crystal potassium niobate nanowire with high length-diameter ratio, good crystallinity and flexibility can be obtained only by hydrothermal reaction under proper KOH concentration and high filling degree, and the reaction time of the method is only 8 to 16 hours, so that the efficiency is high and the repeatability is good. The good flexibility can make up the defect that the rigid nanowire cannot be bent, and is further used for preparing a flexible nano device; the high length-diameter ratio and good crystallinity can make up the defects of low specific surface area and the like of the nanowires prepared by other hydrothermal methods, and improve the reaction site concentration, the adsorption property and the like of the potassium niobate nanowires.
Claims (7)
1. The flexible potassium niobate nanowire is characterized in that the diameter of the nanowire is 5-30nm, and the ratio of the length to the diameter of the nanowire is more than 50.
2. A method for preparing the potassium niobate ultrafine nanowires of claim 1, characterized by comprising the following steps:
step 1: weighing niobium pentoxide and potassium hydroxide, adding water, and uniformly mixing to ensure that the concentration of the potassium hydroxide is 5-8.5 mol/L;
step 2: adding the mixed solution prepared in the step 1 into a reaction kettle, wherein the volume filling amount is 85-95%, sealing, raising the temperature to 180-240 ℃ by programming, keeping the temperature for 8-16 hours, and cooling; filtering, washing and drying.
3. The method according to claim 2, wherein the molar ratio of potassium hydroxide to niobium pentoxide in step 1 is (85-100): 1.
4. The method according to claim 2, wherein the temperature programming speed in step 2 is 1 to 5 ℃/min.
5. The method according to claim 2, wherein the filtration step in the step 2 is carried out using a microfiltration membrane having a pore size of 0.1 μm.
6. The method according to claim 2, wherein the water in step 1 is deionized water; the washing step in the step 2 is washing by using deionized water and absolute ethyl alcohol.
7. The method according to claim 2, wherein the drying temperature in step 2 is 45 to 100 ℃.
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