CN103864033A - Method for preparing titanium nitride (TiN) material - Google Patents
Method for preparing titanium nitride (TiN) material Download PDFInfo
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- CN103864033A CN103864033A CN201410121084.4A CN201410121084A CN103864033A CN 103864033 A CN103864033 A CN 103864033A CN 201410121084 A CN201410121084 A CN 201410121084A CN 103864033 A CN103864033 A CN 103864033A
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Abstract
The invention relates to a method for preparing a titanium nitride (TiN) nano-material with a three-dimensional communicated pore passage structure. According to the method, firstly, titania nanotubes, which have microcosmic morphologies and hierarchical structures similar to those of a cellulosic material, are prepared through taking the natural cellulosic material as a template and taking tetrabutyl titanate as a titanium precursor, and then, the TiN nano-material with the three-dimensional communicated pore passage structure is prepared in a high-temperature (1,100-1,300 DEG C) tubular furnace by a magnesium thermal reduction method through taking magnesium metal as a reductant. The TiN nano-material prepared by using the method has the complicated three-dimensional communicated pore passage structure, uniform-thickness tube walls and relatively high specific surface area and pore volume, so that the TiN nano-material with the complicated three-dimensional communicated pore passage structure is expected to have good application prospects in the fields of catalysis and adsorptive separation.
Description
The present patent application is application number 201210241535.9, the applying date on 07 12nd, 2012, the divisional application of denomination of invention " a kind of titanium nitride nano material and preparation method with three-dimensional communication pore passage structure ".
Technical field
The invention belongs to technical field of material, be specifically related to a kind of preparation method of titanium nitride nano material.
Background technology
Titanium nitride (TiN) is a kind of transition metal nitride, there is B1 – NaCl type crystal structure, because of its excellent physics and chemistry character, for example high rigidity, high-melting-point, good specific conductivity, thermal conductivity and erosion resistance, and high chemical stability, there is important using value in engineering application aspect, therefore receive investigator's very big concern.In recent years, about the existing more research of research of nanostructure TiN, but existing report is mainly around preparation and the property research of titanium nitride nano particle and titanium nitride membrane, research about three-dimensional nitride nano-material is little, and the unicity of resulting materials microtexture and pattern has limited its application in industry and field of engineering technology.The biological tissue that biological template nano materials refers to have suitable construction is template, utilizes self-assembly and space confinement effect, forms the both nano material of fixed structure or the process of nanostructure by the method such as physics, chemistry.The structural unit of many biological tissues is all in nanometer range, and these biological structure unit with nanoscale or nano aperture all can be used as template and prepare nano material.Due to the various advantages (size of Nano grade, diversified profile, nature rich content and environmental friendliness etc.) of biomolecules, take biological tissue as template, the artificial material nano material by self assembly with complicated nanostructure and microscopic appearance is an extremely potential research direction.As the natural fiber element material of the important a member of biological template, the abundantest in distributed in nature, there is unique and complex three-dimensional hierarchical structure, application natural fiber element material is the functional materials that template and skeleton preparation have multilayered structure and pattern, is one and prepares easy, the low cost of functional materials and the synthetic shortcut of environmental protection.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of the titanium nitride nano material with three-dimensional communication pore passage structure.
Method provided by the invention, specifically comprises the following steps, a kind of preparation method of the titanium nitride nano material with three-dimensional communication pore passage structure:
(1) under whipped state, successively 36% concentrated hydrochloric acid and tetrabutyl titanate are joined in organic solvent, continue to stir 3 h and make TiO 2 sol.Wherein, raw material is followed tetrabutyl titanate: dense HCl: the mass ratio of organic solvent=7:5:50 ~ 100; Described organic solvent is dehydrated alcohol or dehydrated alcohol/toluene (volume ratio 1:1) mixed solution.
(2) natural fiber prime modulus plate is dipped in above-mentioned solution, leaves standstill after 3 ~ 12 h and take out, deionized water wash number all over after put into 40 ~ 65 ° of C loft drier dried overnight; Dried sample is raised to 450 ~ 600 ° of C roasting 4 ~ 6 h with the temperature rise rate of 2 ° of C/min and removes template and obtain titania nanotube material; Described natural fiber prime modulus plate is the one in quantitative paper, hospital gauze, absorbent cotton.
(3) under room temperature, in nitrogen atmosphere by above gained titania nanotube and MAGNESIUM METAL particle be placed in respectively two ends, left and right in homemade stainless steel cauldron according to the mol ratio of 1:2.5 ~ 4, do not contact each other; Inflated with nitrogen in reactor is rapidly heated to (10 ° of C/min of temperature rise rate) to 1100 ~ 1300 ℃ of maintenance 2 ~ 5 h, rear cool to room temperature except its sealing being put into after net air to tube furnace;
(4) reaction product is processed to 6 ~ 10 h with 1 ~ 2 M dilute acid solution and remove by product MgO, obtain target product.Described diluted acid is dilute hydrochloric acid or rare nitric acid.
The present invention has following beneficial effect:
The titanium nitride material that the present invention prepares is the nano pore structure with three-dimensional communication, aspect mass transfer, has advantage.Target product has larger specific surface area and pore volume, and traditional solid nitride powder Particle Phase ratio, has more wide application prospect in catalysis and fractionation by adsorption field.
Accompanying drawing explanation
Fig. 1 be preparation have three-dimensional communication pore passage structure the SEM figure of titanium nitride nano material.
Fig. 2 be preparation have three-dimensional communication pore passage structure the XRD figure of titanium nitride nano material.
Embodiment
Below by embodiment, the present invention is further described.
Embodiment 1
(1) under whipped state, successively concentrated hydrochloric acid and tetrabutyl titanate are joined in dehydrated alcohol/toluene mixture (volume ratio 1:1), continue to stir 3 h.Wherein, raw material is followed tetrabutyl titanate: the mass ratio of dense HCl: dehydrated alcohol/toluene=7:5:100;
(2) absorbent cotton is dipped in above-mentioned solution, after standing 3 h, takes out, by deionized water wash number time, put into 65 ° of C loft drier dried overnight; Dried sample is raised to 550 ° of C roasting 5 h with the temperature rise rate of 2 ° of C/min and removes template and make titania nanotube material;
(3) under room temperature, in nitrogen atmosphere, gained titania nanotube and MAGNESIUM METAL particle are placed in respectively to two ends, left and right in homemade stainless steel cauldron according to the mol ratio of 1:4, do not contact each other; The 2 h Ex-alls of inflated with nitrogen in reactor are wherein sealed after air, put into tube furnace with the temperature rise rate of 10 ° of C/min be rapidly heated to 1300 ℃ keep 2 h, after be cooled to room temperature;
(4) reaction product is processed to 6 h with 2 M diluted hydrochloric acid aqueous solutions and remove by product MgO, obtain target product.
Embodiment 2
(1) under whipped state, successively concentrated hydrochloric acid and tetrabutyl titanate are joined in dehydrated alcohol/toluene mixture (volume ratio 1:1), continue to stir 3 h.Wherein, raw material is followed tetrabutyl titanate: the mass ratio of dense HCl: dehydrated alcohol/toluene=7:5:100;
(2) medical gauze is dipped in above-mentioned solution, after standing 3 h, takes out, by deionized water wash number time, put into 65 ° of C loft drier dried overnight; Dried sample is raised to 550 ° of C roasting 5 h with the temperature rise rate of 2 ° of C/min and removes template and make titania nanotube material;
(3) under room temperature, in nitrogen atmosphere, gained titania nanotube and MAGNESIUM METAL particle are placed in respectively to two ends, left and right in homemade stainless steel cauldron according to the mol ratio of 1:4, do not contact each other; The 2 h Ex-alls of inflated with nitrogen in reactor are wherein sealed after air, put into tube furnace with the temperature rise rate of 10 ° of C/min be rapidly heated to 1100 ℃ keep 2 h, after be cooled to room temperature;
(4) reaction product is processed to 6 h with 2 M diluted hydrochloric acid aqueous solutions and remove by product MgO, obtain target product.
Embodiment 3
(1) under whipped state, successively concentrated hydrochloric acid and tetrabutyl titanate are joined in dehydrated alcohol, continue to stir 3 h.Wherein, tetrabutyl titanate: the mass ratio of dense HCl: dehydrated alcohol=7:5:50;
(2) common use for laboratory quantitative paper is dipped in above-mentioned solution, after standing 3 h, takes out, by deionized water wash number time, put into 65 ° of C loft drier dried overnight; Dried sample is raised to 550 ° of C roasting 5 h with the temperature rise rate of 2 ° of C/min and removes template and obtain titania nanotube material;
(3) under room temperature, in nitrogen atmosphere, gained titania nanotube and MAGNESIUM METAL particle are above placed in respectively to two ends, left and right in homemade stainless steel cauldron according to the mol ratio of 1:2.5, do not contact each other; The 2 h Ex-alls of inflated with nitrogen in reactor are wherein sealed after air, put into tube furnace with the temperature rise rate of 10 ° of C/min be rapidly heated to 1300 ℃ keep 2 h, after be cooled to room temperature;
(4) reaction product is processed to 10 h with 1 M diluted nitric acid aqueous solution and remove by product MgO, obtain target product.
Claims (1)
1. a preparation method for titanium nitride material, is characterized in that, according to the following steps:
(1) under whipped state, successively 36% concentrated hydrochloric acid and tetrabutyl titanate are joined in dehydrated alcohol/toluene mixture (volume ratio 1:1), continue to stir 3 h left and right and make TiO 2 sol; Wherein, tetrabutyl titanate: the mass ratio of dense HCl: dehydrated alcohol/toluene=7:5:50;
(2) absorbent cotton is dipped in above-mentioned solution, after standing 12h, takes out, by deionized water wash number time, put into 40 ° of C loft drier dried overnight; Dried sample is raised to approximately 600 ° of C roasting 6 h with the temperature rise rate of 2 ° of C/min and removes template and obtain titania nanotube material;
(3) under room temperature, in nitrogen atmosphere, gained titania nanotube and MAGNESIUM METAL particle are above placed in respectively to two ends, left and right in stainless steel cauldron according to the mol ratio of 1:4, do not contact each other; The 2 h Ex-alls of inflated with nitrogen in reactor are wherein sealed after air, put into tube furnace and be rapidly heated to 1100 ℃ and keep up and down 5 h with the temperature rise rate of 10 ° of C/min, after be cooled to room temperature;
(4) reaction product is processed to 10 h with 1 M diluted nitric acid aqueous solution and remove by product MgO, obtain target product.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210241535.9A CN102701163B (en) | 2012-07-12 | 2012-07-12 | Titanium nitride nanometer material having three-dimensional connected pore channel structure and preparation method of titanium nitride nanometer material |
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| CN201210241535.9A Division CN102701163B (en) | 2012-07-12 | 2012-07-12 | Titanium nitride nanometer material having three-dimensional connected pore channel structure and preparation method of titanium nitride nanometer material |
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| CN103864033B CN103864033B (en) | 2016-01-20 |
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| CN201410121032.7A Expired - Fee Related CN103864032B (en) | 2012-07-12 | 2012-07-12 | A kind of preparation method of nano material |
| CN201410121084.4A Expired - Fee Related CN103864033B (en) | 2012-07-12 | 2012-07-12 | A kind of preparation method of titanium nitride material |
| CN201210241535.9A Expired - Fee Related CN102701163B (en) | 2012-07-12 | 2012-07-12 | Titanium nitride nanometer material having three-dimensional connected pore channel structure and preparation method of titanium nitride nanometer material |
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| CN103450475B (en) * | 2013-09-13 | 2015-10-21 | 中北大学 | The preparation method of core-shell structural conductive polyaniline/Co3O4 powder |
| CN103736475B (en) * | 2014-01-08 | 2015-08-19 | 国家纳米科学中心 | A kind of three-dimensional porous titanium dioxide nano tube catalyst, preparation method and its usage |
| CN105502316B (en) * | 2016-01-30 | 2018-01-12 | 武汉科技大学 | A kind of nitride powder based on low temperature liquid polymerization process and preparation method thereof |
| CN107675483B (en) * | 2017-09-21 | 2019-08-06 | 东华大学 | A kind of preparation method of the titania nanotube based on click chemistry/cotton fabric catalysis material |
| CN108213461B (en) * | 2017-12-12 | 2021-07-16 | 昆明理工大学 | Preparation method of nano-grade noble metal material |
| CN108298957A (en) * | 2018-02-06 | 2018-07-20 | 叶剑 | A kind of preparation method of 3 D stereo nano material |
| CN110606487A (en) * | 2019-10-16 | 2019-12-24 | 大连理工大学 | Honeycomb three-dimensional porous MXene with controllable pore diameter and general synthesis method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101811677A (en) * | 2010-05-06 | 2010-08-25 | 东华大学 | Method for preparing hollow porous quadruped titanium nitride |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811677A (en) * | 2010-05-06 | 2010-08-25 | 东华大学 | Method for preparing hollow porous quadruped titanium nitride |
Non-Patent Citations (2)
| Title |
|---|
| HAIQING HUANG等: ""Tubular structured hierarchical mesoporous titania material derived from natural cellulosic substances and application as photocatalyst for degradation of methylene blue"", 《MATERIALS RESEARCH BULLETIN》 * |
| 刘效艳等: ""天然纤维素为模板的氮化钛纳米管的制备"", 《中国化学会第28届学术年会第4分会场摘要集》 * |
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| CN103864033B (en) | 2016-01-20 |
| CN102701163B (en) | 2014-03-19 |
| CN103864032B (en) | 2015-09-23 |
| CN103864032A (en) | 2014-06-18 |
| CN103864031B (en) | 2015-07-22 |
| CN103864031A (en) | 2014-06-18 |
| CN102701163A (en) | 2012-10-03 |
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