CN110483043A - A kind of simple and easy method preparing function ceramics niobium potassium compound oxide nano wire - Google Patents
A kind of simple and easy method preparing function ceramics niobium potassium compound oxide nano wire Download PDFInfo
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- C04B35/495—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
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Abstract
The invention belongs to nano material and field of nanometer technology, and in particular to easily prepare function ceramics niobium potassium compound oxide K to a kind of6Nb10.8O30The method of nano wire, which comprises the following steps: (1) by K2CO3、Nb2O5, KCl is according to certain molar ratio weighing and mixing；(2) by mixture ball milling or grinding 1h, and slurry is kept the temperature to 8-12h drying between 70-75 DEG C；(3) will dry it is powder sintered, with the heating rate of 5-10 DEG C/min, in 1000-1100 DEG C of heat preservation 3h, furnace cooling；(4) deionized water of sintered product heat is cleaned, and keeps the temperature 8-12h drying between 70-75 DEG C, finally obtain target product.Invention describes a kind of low in cost, simple process, suitable for the method for mass production niobium potassium compound oxide nano wire, product can be used for the fields such as lithium ion battery negative material, catalysis material.
Description
Technical field
The invention belongs to nano material and field of nanometer technology, and in particular to answer to a kind of function ceramics potassium that easily prepares
Close oxide K6Nb10.8O30The method of nano wire.
Background technique
As a kind of new K2O-Nb2O5Binary system ferroelectric phase, K6Nb10.8O30With special crystal space structure.Root
According to theoretical prediction and experimental verification, K6Nb10.8O30This function ceramics can be used for lithium ion battery negative material, and can be effective
Decomposing organic matter dyestuff, so K6Nb10.8O30The preparation method and performance study of material are gradually of concern.
The safety of lithium ion battery has been a concern, in order to enable lithium ion battery reaches Thermodynamically stable, research
The unremitting redox potential of finding of persons is greater than the negative electrode material of 1.0V (relative to Li+/ Li redox electronics to), with full
The fermi level of sufficient negative electrode material can be lower than the condition of lithium metal fermi level 1.0eV.By the study found that Nb5+/Nb4+Oxygen
Change goes back primary electron to can satisfy above-mentioned condition, and electrode potential lower than studying more lithium titanate (Li at present4Ti5O12)
Potential (1.5V), to improve cell voltage and energy while the safety that ensure that battery.K6Nb10.8O30It is one
The material of structure of the kind based on tungsten bronze mine, since there are octahedral connections that vertex is shared in crystal space structure, so that
There are the channels that section is pentagon, quadrangle and triangle along c-axis direction for structure cell, so K6Nb10.8O30Material removing can
To provide Nb5+/Nb4+Except redox electronics pair, the channel of lithium ion transport can also be provided, is conducive to inside battery and reacts
Normal orderly progress.Secondly, K6Nb10.8O30Material is also used as catalysis material.It is surveyed according to ultraviolet specrophotometer
Examination, K6Nb10.8O30The absorption peak of material is about in 425nm or so, corresponding band-gap energy about 2.92eV.Under the irradiation of ultraviolet light,
The dyestuff Acid Red G for being widely used in fabric, drug, plastics etc. can be decomposed.It can be seen that K6Nb10.8O30Material has uniqueness
Structure make it have widely applied potentiality.Currently, about K6Nb10.8O30The preparation method of material is concentrated mainly on solid phase method
The methods of with wet chemistry method.Solid phase synthesis needs that high pressure is undergone to press making powder blank, long-time high-temperature calcination and pole slow cool down speed
Processes, the synthesis cycles such as degree control are longer；In the reactant of wet chemistry method a variety of organic including citric acid hydrochloric acid or
Inorganic reagent, operability are smaller.Therefore, seek the big preparation method synthesis of one kind low in cost, simple process, output
K6Nb10.8O30Material become it is significant and it is necessary to the problem of.
Summary of the invention
The technical problems to be solved by the present invention are: in order to solve existing to prepare function ceramics K6Nb10.8O30Product
The problem of complex technical process, provide it is a kind of it is low in cost, simple process, be suitable for mass production K6Nb10.8O30Nano wire
Method.The present invention solves its technical problem using following technical scheme:
Preparation K provided by the invention6Nb10.8O30The method of nano wire, specifically: by molten based on topochemical reaction
Salt method, reactant adjustment and the control of process conditions prepare K6Nb10.8O30Nano wire.This method is specially using including following
The method of step:
(1) by potassium carbonate, niobium pentaoxide, potassium chloride raw material according to 1.5:3:30 or 0.8:3:30 molar ratio weighing simultaneously
Mixing；
(2) mixture material is poured into zirconia ball grinding jar, is mixed with zirconium oxide balls, pour into dehydrated alcohol to flooding
Mixture, ball milling 1h；Or agate mortar is used, pour into appropriate dehydrated alcohol, hand lapping 1h.Mixed slurry is taken out, and
8-12h is kept the temperature under the conditions of 70-75 DEG C until drying；
(3) resulting drying white powder is placed in Muffle furnace, 1000-1100 is warming up to the speed of 5-10 DEG C/min
DEG C, and 3h is kept the temperature at this temperature, furnace cooling obtains sintering powder；
(4) sintering powder is cleaned, is cleaned 5-8 times using hot deionized water, and examine cleaning solution with silver nitrate solution
In no longer have chloride ion until.8-12h is kept the temperature under the conditions of 70-75 DEG C for resulting cleaning powder until drying.
The present invention has the advantages that following main compared with prior art:
1) reactant feed is cheap and easy to get；
2) preparation process does not generate noxious material, not can cause environmental pollution；
3) fused salt used in experimentation can recycle, and reusable；
4) entire experimental implementation process is simple and easy, favorable reproducibility；
5) it is suitable for high-volume industrial production.The K of synthesis6Nb10.8O30Nano wire has extensive purposes, such as prepares lithium
Ion battery cathode material, for fields such as degradation of organic substances dyestuffs.
Detailed description of the invention
Fig. 1 is K6Nb10.8O30The XRD diagram of nano wire.
Fig. 2 is K6Nb10.8O30The low power SEM of nano wire schemes.
Fig. 3 is K6Nb10.8O30The high power SEM of nano wire schemes.
Fig. 4 is K6Nb10.8O30The ICP testing result table 1 of nano wire.
Specific embodiment
In order to better understand the present invention, below with reference to the embodiment content that the present invention is further explained, but it is of the invention
Content be not limited solely to the following examples.
Embodiment 1
(1) by following three kinds of raw materials: potassium carbonate, niobium pentaoxide and potassium chloride, according to molar ratio K2CO3: Nb2O5: KCl
The ratio of=1.5:3:10 mixes.The specific quality that weighs is respectively as follows: 1.6151g, 6.1536g, 17.3372g；
(2) the zirconium oxide ball milling added with zirconium oxide balls (weight ratio 3mm abrading-ball: 5mm abrading-ball=2:1) is poured the mixture into
In tank, alcohol is poured into later to flooding mixture 10mm or so.Ball grinder with honest material is put into using planetary ball mill, choosing
Revolving speed is 250r/min, ball milling 1 hour；Slurry after ball milling is taken out, and in oven drying.Choosing drying temperature is 70 DEG C,
It is completely dried to product within heat preservation 12 hours；
(3) drying powder is collected, and poured into alumina crucible.Crucible is placed in batch-type furnace later, according to 5 DEG C/
The heating rate of min rises to 1000 DEG C, furnace cooling after heat preservation 3 hours；
(4) deionized water (> 80 DEG C) for being sintered powder heat is cleaned 8 times, and with the silver nitrate (AgNO of 0.1mol/L3)
Solution carries out Cl-The inspection of ion, until not having Cl-Until ion.Powder after cleaning is dry.Choosing drying temperature is 70
DEG C, 12 hours are kept the temperature, K is obtained6Nb10.8O30Nanowire product.The X-ray diffraction analysis the result is shown in Figure 1 of product.
Embodiment 2
(1) by following three kinds of raw materials: potassium carbonate, niobium pentaoxide and potassium chloride, according to molar ratio K2CO3: Nb2O5: KCl
The ratio of=1.5:3:10 mixes.The specific quality that weighs is respectively as follows: 1.6151g, 6.1536g, 17.3372g；
(2) the zirconium oxide ball milling added with zirconium oxide balls (weight ratio 3mm abrading-ball: 5mm abrading-ball=2:1) is poured the mixture into
In tank, alcohol is poured into later to flooding mixture 10mm or so.Ball grinder with honest material is put into using planetary ball mill, choosing
Revolving speed is 300r/min, ball milling 1 hour；Slurry after ball milling is taken out, and in oven drying.Choosing drying temperature is 70 DEG C,
It is completely dried to product within heat preservation 8 hours；
(3) drying powder is collected, and poured into alumina crucible.Crucible is placed in batch-type furnace later, according to 8 DEG C/
The heating rate of min rises to 1000 DEG C, furnace cooling after heat preservation 3 hours；
(4) deionized water (> 80 DEG C) for being sintered powder heat is cleaned 7 times, and with the silver nitrate (AgNO of 0.1mol/L3)
Solution carries out Cl-The inspection of ion, until not having Cl-Until ion.Powder after cleaning is dry.Choosing drying temperature is 70
DEG C, 8 hours are kept the temperature, K is obtained6Nb10.8O30Nanowire product.The pattern result of product is shown in Fig. 2.
Embodiment 3
(1) by following three kinds of raw materials: potassium carbonate, niobium pentaoxide and potassium chloride, according to molar ratio K2CO3: Nb2O5: KCl
The ratio of=1.5:3:10 mixes.The specific quality that weighs is respectively as follows: 1.6151g, 6.1536g, 17.3372g；
(2) the zirconium oxide ball milling added with zirconium oxide balls (weight ratio 3mm abrading-ball: 5mm abrading-ball=2:1) is poured the mixture into
In tank, alcohol is poured into later to flooding mixture 10mm or so.Ball grinder with honest material is put into using planetary ball mill, choosing
Revolving speed is 300r/min, ball milling 1 hour；Slurry after ball milling is taken out, and in oven drying.Choosing drying temperature is 70 DEG C,
It is completely dried to product within heat preservation 12 hours；
(3) drying powder is collected, and poured into alumina crucible.Crucible is placed in batch-type furnace later, according to 10 DEG C/
The heating rate of min rises to 1100 DEG C, furnace cooling after heat preservation 3 hours；
(4) deionized water (> 80 DEG C) for being sintered powder heat is cleaned 6 times, and with the silver nitrate (AgNO of 0.1mol/L3)
Solution carries out Cl-The inspection of ion, until not having Cl-Until ion.Powder after cleaning is dry.Choosing drying temperature is 70
DEG C, 12 hours are kept the temperature, K is obtained6Nb10.8O30Nanowire product.The pattern result of product is shown in Fig. 3.
Embodiment 4
(1) by following three kinds of raw materials: potassium carbonate, niobium pentaoxide and potassium chloride, according to molar ratio K2CO3: Nb2O5: KCl
The ratio of=0.8:3:10 mixes.The specific quality that weighs is respectively as follows: 0.8614g, 6.1536g, 17.3372g；
(2) it pours the mixture into added in agate mortar, pouring into suitable alcohols, hand lapping 1 hour；By the slurry after ball milling
Material takes out, and in oven drying.Choosing drying temperature is 75 DEG C, is completely dried to product within heat preservation 8 hours；
(3) drying powder is collected, and poured into alumina crucible.Crucible is placed in batch-type furnace later, according to 5 DEG C/
The heating rate of min rises to 1100 DEG C, furnace cooling after heat preservation 3 hours；
(4) deionized water (> 80 DEG C) for being sintered powder heat is cleaned 8 times, and with the silver nitrate (AgNO of 0.1mol/L3)
Solution carries out Cl-The inspection of ion, until not having Cl-Until ion.Powder after cleaning is dry.Choosing drying temperature is 75
DEG C, 8 hours are kept the temperature, K is obtained6Nb10.8O30Nanowire product.The X-ray diffraction analysis the result is shown in Figure 1 of product.
Embodiment 5
(1) by following three kinds of raw materials: potassium carbonate, niobium pentaoxide and potassium chloride, according to molar ratio K2CO3: Nb2O5: KCl
The ratio of=0.8:3:10 mixes.The specific quality that weighs is respectively as follows: 0.8614g, 6.1536g, 17.3372g；
(2) it pours the mixture into added in agate mortar, pouring into suitable alcohols, hand lapping 1 hour；By the slurry after ball milling
Material takes out, and in oven drying.Choosing drying temperature is 75 DEG C, is completely dried to product within heat preservation 8 hours；
(3) drying powder is collected, and poured into alumina crucible.Crucible is placed in batch-type furnace later, according to 8 DEG C/
The heating rate of min rises to 1000 DEG C, furnace cooling after heat preservation 3 hours；
(4) deionized water (> 80 DEG C) for being sintered powder heat is cleaned 7 times, and with the silver nitrate (AgNO of 0.1mol/L3)
Solution carries out Cl-The inspection of ion, until not having Cl-Until ion.Powder after cleaning is dry.Choosing drying temperature is 75
DEG C, 10 hours are kept the temperature, K is obtained6Nb10.8O30Nanowire product.The component ratio of product is shown in Table 1.
Claims (12)
1. a kind of prepare function ceramics niobium potassium compound oxide K6Nb10.8O30The simple and easy method of nano wire, which is characterized in that including
Following steps:
(1) potassium resource raw material, niobium source raw material and fused salt raw material through over-stoichiometric are mixed according to a certain percentage, is mixed
Object.
(2) mixture obtained in step (1) is placed in ethanol medium with zirconia ball grinding jar ball milling or is ground using agate
Alms bowl is ground 1 hour, dries ball milling slurry to obtain powder.
(3) drying powder obtained in step (2) is placed in batch-type furnace, heats up according to certain heating rate, uses later
Higher than the temperature of fused salt fusing, subsequent furnace cooling obtains reaction product.
(4) deionized water of reaction product heat obtained in step (3) is cleaned, and dry, finally obtains target product
K6Nb10.8O30Nano wire.
2. a kind of function ceramics K is prepared according to claim 16Nb10.8O30The simple and easy method of nano wire, feature exist
In: potassium resource raw material used in step (1) is potassium carbonate.Niobium source raw material used is niobium pentaoxide.Fused salt used is chlorine
Change potassium.
3. a kind of function ceramics K is prepared according to claim 16Nb10.8O30The simple and easy method of nano wire, feature exist
In: step (1) described raw material mixes according to a certain percentage refers to potassium carbonate, niobium pentaoxide and sodium chloride according to molar ratio sequentially
It is mixed for the ratio of 1.5:3:10 or 0.8:3:10.
4. a kind of function ceramics K is prepared according to claim 16Nb10.8O30The simple and easy method of nano wire, feature exist
In: ethyl alcohol described in step (2) is dehydrated alcohol.
5. a kind of function ceramics K is prepared according to claim 16Nb10.8O30The simple and easy method of nano wire, feature exist
In: ball milling method described in step (2) is to fall later in the zirconia ball grinding jar poured the mixture into added with zirconium oxide balls
Enter dehydrated alcohol.Using planetary ball mill, revolving speed 250-400r/min, ball milling 1 hour.
6. a kind of function ceramics K is prepared according to claim 16Nb10.8O30The simple and easy method of nano wire, feature exist
In: lapping mode described in step (2) is to pour the mixture into agate mortar, dehydrated alcohol is poured into, using hand lapping
Mode continues 1 hour.
7. a kind of function ceramics K is prepared according to claim 16Nb10.8O30The simple and easy method of nano wire, feature exist
In: step (2) described stoving process is that baking oven uses 70-75 DEG C, keeps the temperature 8-12 hours.
8. a kind of function ceramics K is prepared according to claim 16Nb10.8O30The simple and easy method of nano wire, feature exist
In: step (3) certain heating rate is 5-10 DEG C/min.
9. a kind of function ceramics K is prepared according to claim 16Nb10.8O30The simple and easy method of nano wire, feature exist
In: step (3) described holding temperature refers to 1000-1100 DEG C, soaking time 3h.
10. a kind of function ceramics K is prepared according to claim 16Nb10.8O30The simple and easy method of nano wire, feature exist
In: step (4) described cleaning process is to be cleaned 6-8 times with hot deionized water, and use AgNO3Reagent detect cleaning solution until
Inspection does not measure Cl-Until ion.
11. a kind of function ceramics K is prepared according to claim 16Nb10.8O30The simple and easy method of nano wire, feature exist
In: step (4) described drying process is that baking oven uses 70-75 DEG C, keeps the temperature 8-12 hours.
12. a kind of function ceramics K is prepared according to claim 16Nb10.8O30The simple and easy method of nano wire, feature exist
In: step (4) the target product K6Nb10.8O30Nano wire macroscopically sees that product is sparse white powder；It is seen on microcosmic,
Product length is about 50 μm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114256365A (en) * | 2021-12-28 | 2022-03-29 | 陕西师范大学 | KNb3O8Nanobelt, preparation method and application thereof in deep ultraviolet photoelectric detection |
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| CN1686939A (en) * | 2005-04-28 | 2005-10-26 | 西北工业大学 | Method for preparing micro crystalline powder of pure potassium strontium niobite |
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2019
- 2019-05-28 CN CN201910448680.6A patent/CN110483043A/en active Pending
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| CN1686939A (en) * | 2005-04-28 | 2005-10-26 | 西北工业大学 | Method for preparing micro crystalline powder of pure potassium strontium niobite |
| CN102992403A (en) * | 2012-10-22 | 2013-03-27 | 北京工业大学 | Method for preparing one-dimensional nano bar-shaped potassium niobate powder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114256365A (en) * | 2021-12-28 | 2022-03-29 | 陕西师范大学 | KNb3O8Nanobelt, preparation method and application thereof in deep ultraviolet photoelectric detection |
| CN114256365B (en) * | 2021-12-28 | 2023-10-24 | 陕西师范大学 | KNb 3 O 8 Nanobelt, preparation method and application thereof in deep ultraviolet photoelectric detection |
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