CN114835150A - Preparation of LaTiO from single precursor 2 Method for producing N-oxynitride - Google Patents
Preparation of LaTiO from single precursor 2 Method for producing N-oxynitride Download PDFInfo
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- CN114835150A CN114835150A CN202210423196.XA CN202210423196A CN114835150A CN 114835150 A CN114835150 A CN 114835150A CN 202210423196 A CN202210423196 A CN 202210423196A CN 114835150 A CN114835150 A CN 114835150A
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- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention discloses a method for preparing LaTiO by using a single precursor 2 A method for preparing N oxynitride belongs to the field of preparation of perovskite structure nitrogen-containing complex semiconductor materials, and mainly relates to three steps, namely synthesis of a bimetallic compound with stoichiometric ratio of La and Ti; secondly, calcining the La and Ti bimetallic compound in air atmosphere to obtain La 2 Ti 2 O 7 (ii) a Finally, La is added 2 Ti 2 O 7 Performing nitridation to obtain LaTiO 2 And N is added. The invention uses a pure bimetallic compound [ La (H) containing La and Ti 2 O) 4 ] 2 [Ti 2 (O 2 ) 2 O(NC 6 H 6 O 6 ) 2 ]To obtain LaTiO 2 Oxide precursor La required for N-oxynitride 2 Ti 2 O 7 The exact stoichiometric ratio of La and Ti can be ensured so that a non-hetero-phase is relatively easily obtainedLaTiO 2 And (4) N product.
Description
Technical Field
The invention relates to the field of preparation of perovskite structure nitrogen-containing complex semiconductor materials, and specifically relates to a method for preparing LaTiO from a single precursor 2 A method of N oxynitride.
Background
In recent years, a bimetallic oxynitride AB (O, N) having a perovskite structure 3 (a ═ Ca, Sr, Ba, La, Ce, Pr, Nd, etc., and B ═ Ti, Nb, Ta, W) are receiving attention from domestic and foreign scholars because of their novel optical, electrical, magnetic, color, and photocatalytic properties. In its crystal structure, the metal atom at the B-position and the O/N atom form B (O, N) 6 The octahedron B is positioned in the center of the octahedron, the metal atoms at the A position are positioned between the octahedron and occupy eight vertexes of a unit cell to form a unique perovskite structure; different from the common ABO 3 Of perovskite structure, AB (O, N) 3 Wherein the O/N atoms are randomly distributed in B (O, N) 6 Octahedron vertexes, and the distribution mode brings diversity of physical and chemical properties. The theoretical band gap of the material is usually between 1.5-2.5 eV, and the material belongs to a typical semiconductor material.
Patent information of similar products refers to the prior patents: CN109928761A, CN109928762A, CN109331853A, CN109928763A, CN113480316A, CN102995053A, CN1062885C, CN112371159A, CN107583661A, etc.
The defects in the prior art are as follows: currently about AB (O, N) 3 The preparation method of (A) is mainly divided into two methods. Firstly, a pure solid phase chemical synthesis method is used for preparing AB (O, N) by grinding and calcining A site metal source and B site metal source at high temperature 3 Precursor oxides such as La 2 Ti 2 O 7 Etc. nitriding to obtain AB (O, N) 3 (ii) a Secondly, preparing A-site metal source and B-site metal source into sol by a sol-gel method, drying, calcining and the like to obtain AB (O, N) 3 Precursor oxide, and nitriding to obtain AB (O, N) 3 . In both of the above methods, it is necessary to carry out a mixing reaction using at least two precursors of the metal source A and the metal source B, and it is difficult to precisely control the stoichiometric ratio of the metal source A and the metal source B so that AB (O, N) 3 The product often contains lessAnd (4) impurity removal.
Disclosure of Invention
The invention aims to provide a method for preparing LaTiO by using a single precursor 2 The method of N oxynitride solves the following technical problems in the prior art: synthesis of LaTiO by the prior art 2 In the case of N oxynitride, it is difficult to precisely control the stoichiometric ratio of the A metal source and the B metal source, so that LaTiO 2 The N oxynitride often contains a small amount of impurities.
The purpose of the invention can be realized by the following technical scheme:
preparation of LaTiO from single precursor 2 The method of N oxynitride mainly involves three steps, firstly, the synthesis of bimetallic compound with La and Ti stoichiometric ratio; secondly, calcining the La and Ti bimetallic compound in air atmosphere to obtain La 2 Ti 2 O 7 (ii) a Finally, La is added 2 Ti 2 O 7 Performing nitridation to obtain LaTiO 2 N, the specific steps are as follows:
(1) bimetallic compound [ La (H) with La and Ti in stoichiometric ratio 2 O) 4 ] 2 [Ti 2 (O 2 ) 2 O(NC 6 H 6 O 6 ) 2 ]The synthesis of (2):
(a) ultrasonically dispersing nitrilotriacetic acid into distilled water;
(b) slowly dripping tetrabutyl titanate into the solution obtained in the step (a), and magnetically stirring for 2 hours;
(c) under the magnetic stirring state, 30% hydrogen peroxide is injected into the solution obtained in the step (b);
(d) filtering the solution obtained in the step (c) to remove insoluble substances to obtain clear filtrate;
(e) adding lanthanum acetate (1.5 water) into the filtrate obtained in the step (d) under stirring, and continuously stirring by magnetic force for half an hour;
(f) filtering the solution obtained in the step (e), and washing a filter cake for multiple times by using warm water and ethanol;
(g) naturally drying the filter cake obtained in the step (f), and grinding to obtain a powder product, namely the powder product containing La and LaBimetallic compound of Ti [ La (H) 2 O) 4 ] 2 [Ti 2 (O 2 ) 2 O(NC 6 H 6 O 6 ) 2 ]；
Wherein the dosage ratio of the nitrilotriacetic acid, the distilled water, the tetrabutyl titanate, the hydrogen peroxide and the lanthanum acetate is 1.09g to 25mL to 2.042g to 3mL to 1.715 g;
(2) calcining treatment of La and Ti bimetallic compound
Heating the [ La (H) obtained in the step (1) in a temperature programming manner 2 O) 4 ] 2 [Ti 2 (O 2 ) 2 O(NC 6 H 6 O 6 ) 2 ]Calcining the compound in air atmosphere to obtain La 2 Ti 2 O 7 Powder;
the calcination procedure is specifically: heating to 900 ℃ at the heating rate of 2-10 ℃/min, and keeping the temperature for 3-5 h; heating to 1200 ℃ at a heating rate of 2-10 ℃/min, preserving heat for 1-3 h, and cooling to room temperature along with the furnace to obtain La 2 Ti 2 O 7 ；
(3)La 2 Ti 2 O 7 Nitriding treatment of
La obtained in the step (2) 2 Ti 2 O 7 Calcining the powder in ammonia atmosphere to obtain LaTiO 2 An N oxynitride powder;
specifically, La obtained in the step (2) is used 2 Ti 2 O 7 Carrying out ammoniation annealing treatment on the powder in an ammonia atmosphere, heating to 900-1100 ℃ at a heating rate of 5-15 ℃/min, preserving heat for 8-20 h, and cooling to room temperature along with the furnace to obtain LaTiO 2 And (4) N powder.
The invention has the beneficial effects that:
the invention uses a pure bimetallic compound [ La (H) containing La and Ti 2 O) 4 ] 2 [Ti 2 (O 2 ) 2 O(NC 6 H 6 O 6 ) 2 ]To obtain LaTiO 2 Oxide precursor La required for N-oxynitride 2 Ti 2 O 7 Can ensure the accurate stoichiometry of La and TiSo as to obtain LaTiO without impurity phase 2 N products, or LaTiO x N y (0<x,y<2, x + y is less than or equal to 3).
Drawings
The invention will be further described with reference to the accompanying drawings.
FIG. 1 is [ La (H) prepared in example 2 O) 4 ] 2 [Ti 2 (O 2 ) 2 O(NC 6 H 6 O 6 ) 2 ]Schematic structure of the compound.
FIG. 2 shows calcination [ La (H) 2 O) 4 ] 2 [Ti 2 (O 2 ) 2 O(NC 6 H 6 O 6 ) 2 ]La obtained from Compound 2 Ti 2 O 7 XRD spectrum of (1).
FIG. 3 shows a La nitride 2 Ti 2 O 7 The obtained LaTiO 2 XRD spectrum of N.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Examples
Preparation of LaTiO from single precursor 2 A method of N oxynitride comprising the steps of:
(1) bimetallic compound [ La (H) with La and Ti in stoichiometric ratio 2 O) 4 ] 2 [Ti 2 (O 2 ) 2 O(NC 6 H 6 O 6 ) 2 ]The synthesis of (2):
(a) ultrasonically dispersing 1.09g of nitrilotriacetic acid into 25mL of distilled water;
(b) slowly dripping 2.042g of tetrabutyl titanate into the solution obtained in the step (a), and magnetically stirring for 2 hours;
(c) under the magnetic stirring state, 3mL of 30% hydrogen peroxide is injected into the solution obtained in the step (b);
(d) filtering the solution obtained in the step (c) to remove insoluble substances to obtain clear filtrate;
(e) adding 1.715g of lanthanum acetate (1.5 water) to the filtrate obtained in step (d) under stirring, and continuing magnetic stirring for half an hour;
(f) filtering the solution obtained in the step (e), and washing a filter cake for multiple times by using warm water and ethanol;
(g) naturally drying the filter cake obtained in the step (f), and grinding to obtain a powder product, namely the bimetallic compound [ La (H) containing La and Ti 2 O) 4 ] 2 [Ti 2 (O 2 ) 2 O(NC 6 H 6 O 6 ) 2 ]FIG. 1 shows [ La (H) 2 O) 4 ] 2 [Ti 2 (O 2 ) 2 O(NC 6 H 6 O 6 ) 2 ]A schematic diagram of the structure of a compound, in which fig. 1 the corresponding groups can be identified;
(2) calcining treatment of La and Ti bimetallic compound
Heating the [ La (H) obtained in the step (1) in a temperature programming manner 2 O) 4 ] 2 [Ti 2 (O 2 ) 2 O(NC 6 H 6 O 6 ) 2 ]Calcining the compound in air atmosphere to obtain La 2 Ti 2 O 7 Powder;
the calcination procedure is specifically: heating to 900 ℃ at the heating rate of 2-10 ℃/min, and keeping the temperature for 3-5 h; heating to 1200 ℃ at a heating rate of 2-10 ℃/min, preserving heat for 1-3 h, and cooling to room temperature along with the furnace to obtain La 2 Ti 2 O 7 (ii) a Shown as La in FIG. 2 2 Ti 2 O 7 The XRD spectrum of the prepared La is confirmed 2 Ti 2 O 7 Pure phase;
(3)La 2 Ti 2 O 7 nitriding treatment of
The La obtained in the step (2) 2 Ti 2 O 7 Powder ofCalcining in ammonia atmosphere to obtain LaTiO 2 An N oxynitride powder;
specifically, La obtained in the step (2) is used 2 Ti 2 O 7 Carrying out ammoniation annealing treatment on the powder in an ammonia atmosphere, heating to 900-1100 ℃ at a heating rate of 5-15 ℃/min, preserving heat for 8-20 h, and cooling to room temperature along with the furnace to obtain LaTiO 2 N powder, and LaTiO prepared by the method is shown in figure 3 2 XRD pattern of N powder, thus confirming that LaTiO is prepared 2 And N is pure phase.
In the above process, La element can be replaced by other elements of lanthanide series such as Ce, Pr, Nd and the like to prepare corresponding quaternary titanium-based oxynitride.
The above detailed description section specifically describes the analysis method according to the present invention. It should be noted that the above description is only for the purpose of helping those skilled in the art better understand the method and idea of the present invention, and not for the limitation of the related contents. The present invention may be appropriately adjusted or modified by those skilled in the art without departing from the principle of the present invention, and the adjustment and modification also fall within the scope of the present invention.
Claims (7)
1. Preparation of LaTiO from single precursor 2 The method of N oxynitride is characterized by comprising three steps, firstly, La and Ti are stoichiometrically mixed bimetallic compound [ La (H) 2 O) 4 ] 2 [Ti 2 (O 2 ) 2 O(NC 6 H 6 O 6 ) 2 ]Synthesizing; secondly, calcining the La and Ti bimetallic compound in air atmosphere to obtain La 2 Ti 2 O 7 (ii) a Finally, La is added 2 Ti 2 O 7 Performing nitridation to obtain LaTiO 2 N。
2. Preparation of LaTiO from a single precursor according to claim 1 2 A process for preparing N-oxynitrides, characterized in that La, Ti are stoichiometrically mixed as a bimetallic compound [ La (H) 2 O) 4 ] 2 [Ti 2 (O 2 ) 2 O(NC 6 H 6 O 6 ) 2 ]The synthesis of (a) is specifically as follows:
(a) ultrasonically dispersing nitrilotriacetic acid into distilled water;
(b) slowly dripping tetrabutyl titanate into the solution obtained in the step (a), and magnetically stirring for 2 hours;
(c) under the magnetic stirring state, 30% hydrogen peroxide is injected into the solution obtained in the step (b);
(d) filtering the solution obtained in the step (c) to remove insoluble substances to obtain clear filtrate;
(e) adding lanthanum acetate into the filtrate obtained in the step (d) under the stirring state, and continuously stirring for half an hour by magnetic force;
(f) filtering the solution obtained in the step (e), and washing a filter cake for multiple times by using warm water and ethanol;
(g) naturally drying the filter cake obtained in the step (f), and grinding to obtain a powder product, namely the bimetallic compound [ La (H) containing La and Ti 2 O) 4 ] 2 [Ti 2 (O 2 ) 2 O(NC 6 H 6 O 6 ) 2 ]。
3. Preparation of LaTiO from a single precursor according to claim 2 2 The method for preparing the N-oxynitride is characterized in that the dosage ratio of the nitrilotriacetic acid, the distilled water, the tetrabutyl titanate, the hydrogen peroxide and the lanthanum acetate is 1.09g to 25mL to 2.042g to 3mL to 1.715 g.
4. Preparation of LaTiO from a single precursor according to claim 3 2 A method for producing N oxynitride, characterized in that lanthanum acetate is a 1.5 hydrate.
5. Preparation of LaTiO from a single precursor according to claim 1 2 The method for preparing the N oxynitride is characterized in that the calcining treatment steps of the La and Ti bimetallic compound are as follows:
adopting a temperature programming mode to heat the [ La (H) obtained in the last step 2 O) 4 ] 2 [Ti 2 (O 2 ) 2 O(NC 6 H 6 O 6 ) 2 ]Calcining the compound in air atmosphere to obtain La 2 Ti 2 O 7 And (3) powder.
6. Preparation of LaTiO from a single precursor according to claim 5 2 The method for preparing the N oxynitride is characterized in that the calcination procedure is specifically as follows: heating to 900 ℃ at the heating rate of 2-10 ℃/min, and keeping the temperature for 3-5 h; heating to 1200 ℃ at a heating rate of 2-10 ℃/min, preserving heat for 1-3 h, and cooling to room temperature along with the furnace to obtain La 2 Ti 2 O 7 。
7. Preparation of LaTiO from a single precursor according to claim 1 2 A method of making an N-oxynitride, characterized in that La 2 Ti 2 O 7 The nitriding treatment steps are as follows:
the La obtained in the last step 2 Ti 2 O 7 Carrying out ammoniation annealing treatment on the powder in an ammonia atmosphere, heating to 900-1100 ℃ at a heating rate of 5-15 ℃/min, preserving heat for 8-20 h, and cooling to room temperature along with the furnace to obtain LaTiO 2 And (4) N powder.
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| CN115770602A (en) * | 2022-11-08 | 2023-03-10 | 大连海事大学 | High-entropy nitrogen oxide material and preparation method and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115770602A (en) * | 2022-11-08 | 2023-03-10 | 大连海事大学 | High-entropy nitrogen oxide material and preparation method and application thereof |
| CN115770602B (en) * | 2022-11-08 | 2024-04-19 | 大连海事大学 | High-entropy nitrogen oxide material and preparation method and application thereof |
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