CN106391077A - Method for synthesizing tantalum-based nitride (nitrogen oxide) nanoparticles, and nanoparticles thereof - Google Patents

Method for synthesizing tantalum-based nitride (nitrogen oxide) nanoparticles, and nanoparticles thereof Download PDF

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CN106391077A
CN106391077A CN201510458457.1A CN201510458457A CN106391077A CN 106391077 A CN106391077 A CN 106391077A CN 201510458457 A CN201510458457 A CN 201510458457A CN 106391077 A CN106391077 A CN 106391077A
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tantalum
nitrogen
oxygen
nano particle
salt
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高庆生
杨晓芸
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Jinan University
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Jinan University
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Abstract

The invention belongs to the technical field of nanometer materials, and discloses a method for controllably synthesizing tantalum-based nitride (nitrogen oxide) nanoparticles, and nanoparticles thereof. The method comprises: dissolving a tantalum salt in an organic alcohol, adding an alkaline earth metal salt and an organic nitrogen source, stirring to obtain a precursor, placing into an inert atmosphere, carrying out high temperature calcination, and treating with a hydrochloric acid solution to obtain the tantalum-based nitride (nitrogen oxide) nanoparticles. According to the present invention, the method has advantages of mild condition and environmental protection, and breaks through the safety hazard and the limitation caused by the traditional method using NH3; by simply regulating the nitrogen source consumption, the precise control of the product nitrification degree is achieved; by effectively regulating the density of the empty orbit unoccupied by d in the tantalum, the product has the catalysis property similar to the precious metals; and the obtained nanoparticles have wide application prospects in the fields of benzene hydrogenation, Fischer-Tropsch synthesis, hydrodesulfurization/hydrodenitrification, alcohol decomposition-hydrogen production and other fine chemical industry catalysis reactions, fuel cell electrode catalysis materials, sensors, electrical materials, and other fields.

Description

A kind of method of synthesis tantalum base nitrogen (oxygen) compound nano particle and its nano particle
Technical field
The invention belongs to technical field of nano material, particularly to a kind of controlledly synthesis tantalum base nitrogen (oxygen) compound The method of nano particle and its nano particle.
Background technology
Transition metal nitride with tantalum nitride as representative due to its unique class noble metal electronic structure and Catalytic performance, good heat endurance, become have most over nearly one, 20 years application prospect catalysis material it One.Particularly in recent years quickly going up along with oil price, the energy and resource efficiently and greenization profit Cry grows to even greater heights, photocatalysis performance and the exploitation relating to hydrogen catalysis reaction to nitride and nitrogen oxides Attract attention further.With the exception of this, because such transition metal nitride, nitrogen oxides close Become raw material to be inexpensively easy to get, save noble metal precious resources, reduction catalytic reaction cost also has important Meaning.Metal nitride catalyst is including hydrazine decomposition, NH3Synthesis and decomposition, hydrofinishing, hydro carbons are different Structure, selection hydrogenation, CO2Be widely used with aspects such as CO hydrogenation, F-T synthesis, in the energy and Great potential (Volpe L, Boudart M.Ammonia synthesis is presented in chemical industry catalytic reaction on molybdenum nitride.J.Phys.Chem.1986,9:4874-4877;J.S.J.Hargreaves, Coordination Chemistry Reviews.2013,257,2015-2031;X.J.Lang,X.D.Chen,J. C.Zhao,Chemical Society Reviews.2014,43,473-486;A.Salamat,A.L.Hector,P. Kroll,P.F.McMillan,Coordination Chemistry Reviews.2013,257,2063-2072;N. E.Breese,Structure and Bonding,Crystal Chemistry of Inorganic Nitride,Springer, Berlin,1992;H.Morkoc,S.N.Mohammad,Science.1995,267,51;V.Heine,Phys. Rev.A 1967,153,673;E.Furimsky,Applied Catalysis a-General.2003,240,1-28; A.M.Alexander,J.S.J.Hargreaves,Chem.Soc.Rev.2010,39,4388-4401;Q.S. Gao,N.Liu,S.N.Wang,Y.Tang,Nanoscale.2014,6,14106;F.Monnet,Y. Schuurman,F.C.S.Aires,J.C.Bertolini,C.Mirodatos,Catal.Today.2001,64, 51-58;M.M.O.Thotiyl,T.R.Kumar,S.Sampath,J.Phys.Chem.C.2010,114, 17934-17941;V.Molinari,C.Giordano,M.Antonietti,D.Esposito,J.Am.Chm. Soc.2014,136,1758-1761;F.Cardenas-Lizana,D.Lamey,N.Perret,S. Gomez-Quero,L.Kiwi-Minsker,M.A.Keane,Catalysis Communications.2012, 21,46-51;K.Maeda,K.Domen,Journal of Physical Chemistry C.2007,111, 7851-7861;R.Asahi,T.Morikawa,T.Ohwaki,K.Aoki,Y.Taga,Science.2001, 293,269-271;Q.S.Gao,C.Giordano,M.Antonietti,Small.2011,7,3334-3340;Y. G.Su,J.Y.Lang,L.P.Li,K.Guan,C.F.Du,L.M.Peng,D.Han,X.J.Wang,J. Am.Chem.Soc.2013,135,11433-11436;Q.S.Gao,S.N.Wang,Y.C.Ma,Y.Tang, C.Giordano,M.Antonietti,Angew.Chem.Int.Ed.2012,51,961-965;R.Abe,M. Higashi,K.Domen,J.Am.Chem.Soc.2010,132,11828-11829;Q.S.Gao,C. Giordano,M.Antonietti,Angew.Chem.Int.Ed.2012,51,11740-11744.).For example, In recent years, lot of domestic and foreign scholar was studying metal nitride and its catalytic performance energetically, found single Metal nitride, bimetallic nitride and load type metal nitride are all excellent hydrogenation and catalysis dehydrogenation Agent, in many hydrogen-involved reactions:In the reactions such as F-T synthesis, CO oxidation, CO hydrogenation, NO reduction all Show good catalytic capability.On the other hand, because tantalum base nitrogen oxides and nitride have semiconductor Property, can absorb the visible ray in solar spectrum, and its band structure also can be controlled, this make it Photochemical catalyzing reaction and light degradation organic pollution and inorganic dyestuff industrial aspect are widely used.
In terms of document report, traditional metal nitride synthetic method about can be divided into following a few class:1) Programmed temperature method, to be heated up nitridation presoma by the program setting, but due to temperature high (>750℃), Synthesis condition harshness is it is difficult to realize industrialization.2) thermal decomposition method, using metallo-organic compound or metal The salt of organic compound heat resolve synthesis metal nitride under carrier gas, but to some metals difficult synthesis gold Belong to organic compound and its salt, have limitation.3) solid state reaction, with metal dust, metal oxide, Or slaine is source metal, NaN3Deng for nitrogen source, after solid-state reaction, synthesize metal nitride, but this method The pressure needing is higher, and used nitrogen source is expensive.4) ball-milling method, is logical under certain atmosphere Crossing ball milling makes raw material be sufficiently mixed and refines, reacts, but because the reaction time is long, raw material is difficult to completely anti- Its difficult large-scale use should be made.In addition with electrochemical process, chemical vapour deposition technique, ultrasonic pen synthetic method, The reports such as the ultrasonic waves such as sol-gal process dispersion, but it is little to equally exist yield, reacts insufficient, product grain The difficult problem such as larger (E.Orhan, F.Tessier, R.Marchand, Solid State Sciences.2002,4, 1071-1076;M.Kerlau,O.Merdrignac-Conanec,M.Guilloux-Viry,A.Perrin,Solid State Sciences.2004,6,101-107;J.B.Claridge,A.P.E.York,A.J.Brungs,M.L. H.Green,Chem.Mater.2000,12,132-142;H.Zhao,M.Lei,X.Chen,W.Tang,J. Mater.Chem.2006,16,4407-4412;J.Buha,I.Djerdj,M.Antonietti,M. Niederberger,Chem.Mater.2007,19,3499-3505;Kasahara A,Nukumizu K,Hitoki G,Takata T,Kondo J N,Hara M,Kobayashi H,Domen K.Photoreaetions on LaTIO2N under visible light irradiation.Journal of Physical Chemistry.A.2002,106: 6750-6752;Tessier F,Marehand R.Ternary and higher order rare-earth nitride materials:synthesis and characterization of ionic-covalent oxynitride powders.J. Solid State Chem.2003,171:143-151;Volpe L,Boudart M.Compounds of molybdenum and tungsten with high specific surface area:I.nitrides.J.Solid State Chem.1985,59:332-347;Wise R S,Markel E J.Catalytic NH3decomposition by topotactic molybdenum oxides and nitrides:Effect on temperature programmed γ-Mo2N synthesis.J.Catal.1994,145:335-343.).
Therefore, using efficient, the accurate tantalum base nitrogen oxides prepared of new synthetic method and nitride Performances of Novel Nano-Porous Rice catalyst, is one of the research topic the most interesting in this field current.The tantalum base nitrogen of controlled Nitration synthesis Oxide and the nitride not only gentle environmental protection of reaction condition, and overcome the problem of excessive nitridation, so as to Enough control band structure, secondly outward appearance as smart as a new pin, assumes multicoloured color, transition metal nitrogen oxidation These interesting properties of thing determine it before photocatalysis field and dye industry have potentiality to be exploited and application Scape.However, there is no report in terms of effectively realizing controlled nitridation at present.
Content of the invention
In order to overcome shortcoming and the deficiency of above-mentioned prior art, the primary and foremost purpose of the present invention is that offer one kind can The method of control synthesis tantalum base nitrogen (oxygen) compound nano particle.
Another object of the present invention is to providing tantalum base nitrogen (oxygen) the compound nanometer that said method prepares Grain.The particle diameter of gained nano particle is all in 10nm.
Still a further object of the present invention is to provide above-mentioned tantalum base nitrogen (oxygen) compound nano particle to be catalyzed in fine chemistry industry Application in the fields such as reaction, fuel cell electrode catalyst material, sensor and electricity material.
The purpose of the present invention is realized by following proposal:
A kind of method of controlledly synthesis tantalum base nitrogen (oxygen) compound nano particle, comprises the following steps:
Tantalum salt is dissolved in Organic Alcohol, adds alkali salt and organic nitrogen source, stirring obtains presoma, After being placed in inert atmosphere high temperature roasting, hydrochloric acid solution is processed, and obtains tantalum base nitrogen (oxygen) compound nano particle.
The consumption of described alkali salt and tantalum salt is defined by the mol ratio of alkaline-earth metal ions and tantalum atom, excellent Elect (0.1~10) as:1, more preferably (0.1~5):1.
The consumption of described organic nitrogen source and tantalum salt is defined by the mol ratio of nitrogen and tantalum atom, preferably (1.0~10):1, more preferably (2~7):1.
Described tantalum salt can be at least in tantalic chloride, tantalum pentabromide, tantalum oxide and five ethoxy-tantalum etc. Kind, preferably tantalic chloride.
Described alkali salt can be strontium chloride, strontium carbonate, strontium nitrate, barium chloride, brium carbonate, nitric acid At least one in barium, magnesium chloride, magnesium sulfate and magnesium nitrate etc., preferably strontium chloride.
Described organic nitrogen source can be at least one in urea, cyanamide, dicyanodiamine and melamine etc., It is preferably urea.Described organic nitrogen source preferably adds after alkali salt dissolving.
Described high-temperature roasting preferably refers to roasting 2~10h at 650~850 DEG C, roasts more preferably at 700 DEG C Burn 5h, heating rate is preferably 1~10 DEG C/min.
The product that described hydrochloric acid solution is processed after referring to high-temperature roasting is placed in stirring 24~48h in hydrochloric acid solution, excellent Elect 48h as.Described process using hydrochloric acid solution is to remove unnecessary alkaline-earth metal ions, therefore used Concentration of hydrochloric acid solution can arbitrarily be adjusted, preferably 1mol/L.Described hydrochloric acid solution is preferably used no after processing again Water-ethanol washing repeatedly, is dried, is obtained product after purification.
Described Organic Alcohol is used for providing solution reaction environment, is alcohols solvent commonly used in the art, such as first Alcohol, ethanol, isopropanol etc..
Described stirring obtains presoma, preferably 4~48h is stirred at room temperature, to formation gel system, Obtain presoma.
Described inert atmosphere can be argon gas, nitrogen or helium.
Tantalum base nitrogen (oxygen) the compound nano particle that said method prepares, this grain diameter is 10nm Left and right.
Tantalum base nitrogen oxides that the inventive method prepares and tantalum base nitride benzene hydrogenation, F- T synthesis, The fine chemistry industry catalytic reactions such as hydrodesulfurization/denitrogenation, alcohols decomposing hydrogen-production, and fuel cell electrode catalyst material Have wide practical use in material, sensor, and the field such as electricity material.
The mechanism of the present invention is:
The inventive method mild condition, environmental protection, breach tradition and use NH3The potential safety hazard brought and Limitation, by the consumption of simple regulation and control nitrogen source, realizes product nitridation is precisely controlled, and more Effectively adjust the unoccupied orbital density that the d of tantalum does not occupy, thus making it have the catalytic of similar noble metal Matter.The tantalum base nitrogen oxides that therefore the inventive method prepares and tantalum base nitride close in benzene hydrogenation, Fischer-Tropsch The fine chemistry industry catalytic reactions such as one-tenth, hydrodesulfurization/denitrogenation, alcohols decomposing hydrogen-production, and fuel cell electrode urges Change in the fields such as material, sensor, and electricity material and have wide practical use.
The present invention, with respect to prior art, has such advantages as and beneficial effect:
(1) the inventive method yield is high, reaches more than 95%.
(2) preparation condition of the present invention is simple and easy to control, process conditions low cost, and preparation efficiency is high, product matter Amount and high yield rate, have good application and industrialization prospect.
Brief description
Fig. 1 is X-ray powder diffraction (XRD) figure of product A.
Fig. 2 is transmission electron microscope (TEM) figure of product A.
Fig. 3 is X-ray powder diffraction (XRD) figure of product B.
Fig. 4 is transmission electron microscope (TEM) figure of product B.
Fig. 5 is ESEM (SEM) figure of product A.
Fig. 6 is ESEM (SEM) figure of product B.
Fig. 7 is ESEM (SEM) figure of products C.
Fig. 8 is ESEM (SEM) figure of product D.
Fig. 9 is ESEM (SEM) figure of product E.
Figure 10 is ESEM (SEM) figure of product F.
Figure 11 is ESEM (SEM) figure of product G.
Figure 12 is ESEM (SEM) figure of product H.
Specific embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but the embodiment party of the present invention Formula not limited to this.
In the following example, reagent used is all commercially available.
Embodiment 1
By 0.25g TaCl5(0.7mM) it is dissolved in 2mL methyl alcohol, be subsequently added 0.103g strontium chloride (0.65mM), rear addition 0.084g urea (1.4mM) to be dissolved, is stirred at room temperature 4h to gel Shape.By it in nitrogen stream 700 DEG C of roasting 5h, by the product the obtaining HCl treatment room temperature of 1mol/L Stirring 48h.Product ethanol will be obtained and wash for several times simultaneously suction filtration, 50 DEG C of dryings.Obtain nitrogen tantalum oxide nanometer Grain A (TaON).
Embodiment 2
By 0.25g TaCl5(0.7mM) it is dissolved in 2mL methyl alcohol, be subsequently added 0.103g strontium chloride (0.65mM), rear addition 0.294g urea (4.9mM) to be dissolved, is stirred at room temperature 4h to gel Shape.By it in nitrogen stream 700 DEG C of roasting 5h, by the product the obtaining HCl treatment room temperature of 1mol/L Stirring 48h.Product ethanol will be obtained and wash for several times simultaneously suction filtration, 50 DEG C of dryings.Obtain five nitridation three tantalum nanometer Particle B (Ta3N5).
Embodiment 3
By 0.25g TaCl5(0.7mM) it is dissolved in 2mL methyl alcohol, be subsequently added 0.103g strontium chloride (0.65mM), rear addition 0.084g urea (1.4mM) to be dissolved, is stirred at room temperature 4h to gel Shape.By it in argon gas stream 700 DEG C of roasting 5h, by the product the obtaining HCl treatment room temperature of 1mol/L Stirring 48h.Product ethanol will be obtained and wash for several times simultaneously suction filtration, 50 DEG C of dryings.Obtain nitrogen tantalum oxide nanometer Grain C (TaON).
Embodiment 4
By 0.25g TaCl5(0.7mM) it is dissolved in 2mL methyl alcohol, be subsequently added 0.555g strontium chloride (3.5mM), rear addition 0.084g urea (1.4mM) to be dissolved, is stirred at room temperature 4h to gel Shape.By it in nitrogen stream 700 DEG C of roasting 5h, by the product the obtaining HCl treatment room temperature of 1mol/L Stirring 48h.Product ethanol will be obtained and wash for several times simultaneously suction filtration, 50 DEG C of dryings.Obtain nitrogen tantalum oxide nanometer Grain D (TaON).
Embodiment 5
By 0.25g TaCl5(0.7mM) it is dissolved in 2mL methyl alcohol, be subsequently added 0.01g strontium chloride (0.07 MM), rear addition 0.084g urea (1.4mM) to be dissolved, is stirred at room temperature 4h to gel.Will Its 700 DEG C of roasting 5h in nitrogen stream, the product obtaining is stirred at room temperature with the HCl treatment of 1mol/L 48h.Product ethanol will be obtained and wash for several times simultaneously suction filtration, 50 DEG C of dryings.Obtain nitrogen tantalum oxide nano particle E (TaON).
Embodiment 6
By 0.25g TaCl5(0.7mM) it is dissolved in 2mL methyl alcohol, be subsequently added 0.0665g magnesium chloride (0.7mM), rear addition 0.21g urea (3.5mM) to be dissolved, is stirred at room temperature 4h to gel. By it in nitrogen stream 700 DEG C of roasting 5h, the product obtaining is stirred at room temperature with the HCl treatment of 1mol/L 48h.Product ethanol will be obtained and wash for several times simultaneously suction filtration, 50 DEG C of dryings.Obtain five nitridation three tantalum nano particle F(Ta3N5).
Embodiment 7
By 0.25g TaCl5(0.7mM) it is dissolved in 2mL methyl alcohol, be subsequently added 0.138g brium carbonate (0.7mM), rear addition 0.21g urea (3.5mM) to be dissolved, is stirred at room temperature 4h to gel. By it in nitrogen stream 700 DEG C of roasting 5h, the product obtaining is stirred at room temperature with the HCl treatment of 1mol/L 48h.Product ethanol will be obtained and wash for several times simultaneously suction filtration, 50 DEG C of dryings.Obtain five nitridation three tantalum nano particle G(Ta3N5).
Embodiment 8
By 0.25g TaCl5(0.7mM) it is dissolved in 2mL methyl alcohol, be subsequently added 0.103g strontium chloride (0.65mM), rear addition 0.617g melamine (4.9mM) to be dissolved, is stirred at room temperature 4h To gel.By it in nitrogen stream 700 DEG C of roasting 5h, by the product obtaining with the hydrochloric acid of 1mol/L Reason is stirred at room temperature 48h.Product ethanol will be obtained and wash for several times simultaneously suction filtration, 50 DEG C of dryings.Obtain five nitridations three Tantalum nano particle H (Ta3N5).
Embodiment 9:The observation of nano particle
The nano particle that embodiment 1~8 is prepared is swept using absorbing on ZEISS ULTRA55 instrument Retouch electromicroscopic photograph (SEM), picked-up lens photo (TEM) on JEOL JEM 2100F instrument, Carry out XRD scanning, result is shown in Fig. 1~12 on Bruker D8 type X-ray diffractometer.
From Fig. 1~2, embodiment 1 successfully prepare nanometer particle size be 10nm about nitrogen oxidation Tantalum.And as seen from Figure 5, the nitrogen tantalum oxide that the present invention prepares can be separated into graininess in ethanol.
Fig. 3~4 show embodiment 2 successfully prepare nanometer particle size be 10nm about five nitridation three tantalums. And as seen from Figure 6, five nitridation three tantalums that the present invention prepares have good dispersiveness in ethanol.
Fig. 7 shows all to prepare the nano particle of favorable dispersibility in different atmosphere of inert gases.
Fig. 8~9 show, equally can be prepared by the mol ratio changing the strontium atom using and tantalum atom Nitrogen tantalum oxide nano particle.
Figure 10~11 show, by changing alkali earth metal, can equally prepare five nitridation three tantalum and receive Rice grain.
Figure 12 shows, when nitrogen source changes into melamine, can equally prepare five nitrogen of good dispersion Change three tantalum nano particles.
From the foregoing, it will be observed that the nitrogen tantalum oxide for preparing of the inventive method and five nitridation three tantalum particles are little, therefore, The insertion of N atom causes metal lattice to be expanded, and metal spacing and lattice constant become big, the phase between metallic atom Interreaction force weakens, and produces corresponding d band and shrinks, thus leading to the neighbouring density of states of Fermi energy level again Distribution, valence electron number increases, and structure also changes therewith.This modulation makes transition metal nitride have concurrently covalently The characteristic of compound, ionic crystals and three kinds of materials of transition metal, thus show on catalytic property completely not It is same as its corresponding metal, and there is the property similar to VIII race's noble metal, in hydrazine decomposition, NH3Synthesis and The aspects such as decomposition, hydrofinishing, hydro carbons isomery, selection hydrogenation are widely used.
Meanwhile, to determine it organic in photochemical catalyzing field and light degradation for the property of the semiconductor that it has Pollutant and the using value of inorganic dyestuff industry.Above potential using value is had based on this product, and And preparation condition is simple and easy to control, process conditions low cost, preparation efficiency height, product quality and high yield rate, The nano particle that therefore present invention prepares has good application and industrialization prospect.To the method system Research, not only can provide the energy catalyzed conversion carbides catalytic material with class noble metal performance of novelty Material, and to the synthetic methodology and Catalyst Design of material, there is wide significance.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not subject to above-mentioned reality Apply the restriction of example, the change made under other any Spirit Essences without departing from the present invention and principle, modification, Substitute, combine, simplify, all should be equivalent substitute mode, be included within protection scope of the present invention.

Claims (10)

1. a kind of method of controlledly synthesis tantalum base nitrogen (oxygen) compound nano particle it is characterised in that include with Lower step:Tantalum salt is dissolved in Organic Alcohol, adds alkali salt and organic nitrogen source, stirring obtains forerunner Body, after being placed in inert atmosphere high temperature roasting, hydrochloric acid solution is processed, and obtains tantalum base nitrogen (oxygen) compound nanometer Particle.
2. the method for controlledly synthesis tantalum base nitrogen (oxygen) compound nano particle according to claim 1, It is characterized in that:The consumption of described alkali salt and tantalum salt is with the mol ratio of alkaline-earth metal ions and tantalum atom It is defined, for (0.1~10):1;
The consumption of described organic nitrogen source and tantalum salt is defined by the mol ratio of nitrogen and tantalum atom, for (1.0~ 10):1.
3. the method for controlledly synthesis tantalum base nitrogen (oxygen) compound nano particle according to claim 1, It is characterized in that:The consumption of described alkali salt and tantalum salt is with the mol ratio of alkaline-earth metal ions and tantalum atom It is defined, for (0.1~5):1;
The consumption of described organic nitrogen source and tantalum salt is defined by the mol ratio of nitrogen and tantalum atom, for (2~ 7):1.
4. the method for controlledly synthesis tantalum base nitrogen (oxygen) compound nano particle according to claim 1, It is characterized in that:Described tantalum salt is tantalic chloride, tantalum pentabromide, in tantalum oxide and five ethoxy-tantalum extremely Few one kind;
Described alkali salt be strontium chloride, strontium carbonate, strontium nitrate, barium chloride, brium carbonate, barium nitrate, At least one in magnesium chloride, magnesium sulfate and magnesium nitrate;
Described organic nitrogen source is at least one in urea, cyanamide, dicyanodiamine and melamine.
5. the method for controlledly synthesis tantalum base nitrogen (oxygen) compound nano particle according to claim 1, It is characterized in that:Described tantalum salt is tantalic chloride;Described alkali salt is strontium chloride;Described has Machine nitrogen source is urea.
6. the method for controlledly synthesis tantalum base nitrogen (oxygen) compound nano particle according to claim 1, It is characterized in that:Described high-temperature roasting refers to roasting 2~10h at 650~850 DEG C.
7. the method for controlledly synthesis tantalum base nitrogen (oxygen) compound nano particle according to claim 1, It is characterized in that:Described high-temperature roasting refers to roasting 5h at 700 DEG C, and heating rate is 1~10 DEG C/min.
8. the method for controlledly synthesis tantalum base nitrogen (oxygen) compound nano particle according to claim 1, It is characterized in that:The product that described hydrochloric acid solution is processed after referring to high-temperature roasting is placed in stirring in hydrochloric acid solution 24~48h.
9. a kind of tantalum base nitrogen (oxygen) compound nano particle is it is characterised in that arbitrary according to claim 1~8 Method described in prepares.
10. tantalum base nitrogen (oxygen) compound nano particle according to claim 9 is anti-in fine chemistry industry catalysis Should, the application in fuel cell electrode catalyst material, sensor and electricity material field.
CN201510458457.1A 2015-07-29 2015-07-29 Method for synthesizing tantalum-based nitride (nitrogen oxide) nanoparticles, and nanoparticles thereof Pending CN106391077A (en)

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CN109928762A (en) * 2018-12-21 2019-06-25 中国人民解放军国防科技大学 BaTaO2N-oxynitride powder and double-nitrogen source preparation method thereof
CN109928762B (en) * 2018-12-21 2022-03-15 中国人民解放军国防科技大学 BaTaO2N-oxynitride powder and double-nitrogen source preparation method thereof
CN109928763A (en) * 2019-03-07 2019-06-25 中国人民解放军国防科技大学 Tantalum-based oxynitride nano powder and preparation method thereof
CN109928763B (en) * 2019-03-07 2022-03-29 中国人民解放军国防科技大学 Tantalum-based oxynitride nano powder and preparation method thereof
CN110316706A (en) * 2019-06-06 2019-10-11 武汉大学 A kind of fused salt chemistry method nitrogenizing tantalum pentoxide and its nitridation tantalum pentoxide prepared
CN110316706B (en) * 2019-06-06 2022-10-18 武汉大学 Molten salt chemical method for tantalum pentoxide nitride and tantalum pentoxide prepared by same
CN111790424A (en) * 2020-07-06 2020-10-20 上海交通大学 Photocatalyst with efficient absorption of visible light and preparation method and application thereof
CN111905808A (en) * 2020-07-16 2020-11-10 兰东辉 Graphene-based composite material and preparation method thereof
CN111905795A (en) * 2020-08-27 2020-11-10 杭州洲钜电子科技有限公司 Simple and convenient environment-friendly Ta preparation method3N5Method for preparing photocatalyst
CN113387708A (en) * 2021-06-30 2021-09-14 中国人民解放军国防科技大学 Compact high dielectric barium tantalum oxynitride ceramic and preparation method thereof

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