CN110586151A - Preparation method of ordered mesoporous transition metal nitride - Google Patents
Preparation method of ordered mesoporous transition metal nitride Download PDFInfo
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- 229910052723 transition metal Inorganic materials 0.000 title claims abstract description 25
- -1 transition metal nitride Chemical class 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 15
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 6
- 238000011049 filling Methods 0.000 claims abstract description 5
- 229910001428 transition metal ion Inorganic materials 0.000 claims abstract description 5
- 239000003513 alkali Substances 0.000 claims abstract description 4
- 230000003647 oxidation Effects 0.000 claims abstract description 3
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 8
- 229910000423 chromium oxide Inorganic materials 0.000 claims description 8
- 229910000428 cobalt oxide Inorganic materials 0.000 claims description 8
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims description 8
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 7
- DMTIXTXDJGWVCO-UHFFFAOYSA-N iron(2+) nickel(2+) oxygen(2-) Chemical compound [O--].[O--].[Fe++].[Ni++] DMTIXTXDJGWVCO-UHFFFAOYSA-N 0.000 claims description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002131 composite material Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 5
- 229920002415 Pluronic P-123 Polymers 0.000 claims description 4
- 229910044991 metal oxide Inorganic materials 0.000 claims description 4
- 150000004706 metal oxides Chemical class 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 229910052573 porcelain Inorganic materials 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 229920000428 triblock copolymer Polymers 0.000 claims description 3
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 claims description 2
- 229910001430 chromium ion Inorganic materials 0.000 claims description 2
- 229910001429 cobalt ion Inorganic materials 0.000 claims description 2
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910001453 nickel ion Inorganic materials 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 239000010937 tungsten Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 9
- 230000035484 reaction time Effects 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 238000001816 cooling Methods 0.000 abstract description 2
- 238000009792 diffusion process Methods 0.000 abstract description 2
- 230000002401 inhibitory effect Effects 0.000 abstract description 2
- 230000001737 promoting effect Effects 0.000 abstract description 2
- 230000002194 synthesizing effect Effects 0.000 abstract description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 239000011148 porous material Substances 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 150000003624 transition metals Chemical class 0.000 description 4
- 150000004767 nitrides Chemical class 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 229910000863 Ferronickel Inorganic materials 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910001960 metal nitrate Inorganic materials 0.000 description 1
- 239000012702 metal oxide precursor Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 238000001988 small-angle X-ray diffraction Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002887 superconductor Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 229910009112 xH2O Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/64—Pore diameter
- B01J35/647—2-50 nm
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a preparation method of ordered mesoporous transition metal nitride, which comprises the following steps: filling a silicon dioxide SBA-15 mesoporous template with transition metal ions, removing the template by using alkali after high-temperature oxidation to generate mesoporous oxide with a mesoporous structure, and then performing high-temperature nitridation treatment on the mesoporous oxide to synthesize ordered mesoporous transition metal nitride; the present invention is based on SBA-15 template-derived precursors, useful for various types of TMN materials. In one aspect, by promoting NH3The gas diffusion of (2) can effectively reduce the reaction time, and is beneficial to synthesizing a rigid mesoporous structure with high crystallinity. On the other hand, the rapid nitridation process can save the time for programming heating and cooling at common temperature, thereby inhibiting the closing and collapse of the mesoporous structure.
Description
Technical Field
The invention relates to the field of nano-structure functional materials, in particular to a preparation method of ordered mesoporous transition metal nitride.
Background
Transition Metal Nitrides (TMN) are intermetallic filling compounds produced by insertion of nitrogen into a transition metal lattice, having properties of covalent compounds, ionic crystals and transition metals. TMN has unique physical and chemical properties, such as high strength, strong acid and alkali resistance, high chemical stability, good conductivity, etc., and thus has wide applications in the fields of superhard materials, protective materials, superconductors, and structural materials. In addition, a great deal of research shows that TMN shows good catalytic activity in a plurality of hydrogen-involved reactions, and even has the performance which is not inferior to the performance of noble metals such as Pt, Rh and the like, so that the TMN has important significance for carrying out extensive and intensive research on the formation mechanism, the preparation condition and the catalytic performance of the TMN and developing the application prospect.
It is well known that specific surface area and pore structure have a great influence on catalytic reactions, whereas a large number of metal active sites and increased pore volume are provided by a high specific surface area and a regular pore structure. The preparation of the transition metal nitride is a local regular reaction, and particularly when a material with high specific surface area is synthesized, the transition metal nitride with high specific surface area can be generated under the condition that the crystal structure of a transition metal oxide precursor is not basically damaged by strictly controlling the reaction conditions. However, most of the existing methods for preparing Transition Metal Nitrides (TMN) involve high temperature heating or high pressure for a long time, and high interfacial energy and pressure exist in such reaction systems, so that the porous structure is inevitably aggregated, closed and collapsed during the transformation and recrystallization processes. Therefore, it is very necessary to use a new method to prepare ordered porous TMN with high specific surface area.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects of the prior art: provides a new method for preparing ordered mesoporous transition metal nitride by a rapid nitridation synthesis method. The method is based on SBA-15 template-derived precursors and can be used for various types of TMN materials. In one aspect, by promoting NH3The gas diffusion of (2) can effectively reduce the reaction time, and is beneficial to synthesizing a rigid mesoporous structure with high crystallinity. On the other hand, the rapid nitridation process can save the time for programming heating and cooling at common temperature, thereby inhibiting the closing and collapse of the mesoporous structure.
The technical solution of the invention is as follows: a method for preparing ordered mesoporous transition metal nitride comprises the following steps: filling transition metal ions in a silicon dioxide SBA-15 mesoporous template, removing the template by using alkali after high-temperature oxidation to generate mesoporous oxide with a mesoporous structure, and then performing high-temperature nitridation treatment on the mesoporous oxide to synthesize the ordered mesoporous transition metal nitride.
The transition metal ions are one or more of cobalt ions, tungsten ions, chromium ions, nickel ions and iron ions.
The mesoporous oxide is one or more of cobalt oxide, tungsten oxide, chromium oxide and nickel iron oxide.
The preparation method of the silicon dioxide SBA-15 mesoporous template comprises the following steps:
1) adding a nonionic triblock copolymer Pluronic P123 into hydrochloric acid with the pH value less than 1, and stirring at 30-50 ℃ until the solute is completely dissolved;
2) adding tetraethyl orthosilicate into the solution prepared in the step 1) under the condition of stirring, uniformly mixing and standing for 10-30 h; heating in an oven at 80-90 ℃ for 10-24h under the standing condition, filtering, washing and drying the precipitate obtained by filtering by using deionized water, and finally calcining at the temperature of more than 500 ℃ to obtain the silicon dioxide SBA-15 mesoporous template.
The preparation method of the mesoporous oxide comprises the following steps:
1) adding a silicon dioxide SBA-15 mesoporous template and an oxide precursor into ethanol, uniformly mixing, stirring at room temperature for 30-50min, heating to 60-80 ℃, and evaporating to remove ethanol to obtain a mesoporous silicon composite material;
2) putting the mesoporous silicon composite material into a porcelain boat, heating for 3-4h at the temperature of 250 ℃ in a muffle furnace at 230 ℃, removing the silicon dioxide SBA-15 mesoporous template by using NaOH solution, washing by using deionized water and ethanol, and drying in vacuum at the temperature of 60-80 ℃ to obtain the mesoporous oxide.
The oxide precursor is metal salt corresponding to metal oxide; the metal oxide is one or more of cobalt oxide, chromium oxide, tungsten oxide and nickel iron oxide.
The invention has the beneficial effects that: the invention can synthesize a series of binary and ternary TMN materials (Co) within 30minN, WN, CrN and Ni3FeN) and avoids pore collapse, and a perfect mesoporous structure is maintained, so that the catalyst has a high specific surface area and can provide more active sites in a catalytic reaction. The successful preparation of the series of materials shows that the invention has universality and wide application prospect. In addition, the preparation method has the advantages of simple operation, simple equipment, uniform product and short overall reaction time.
Drawings
FIG. 1: the X-ray diffraction pattern of the example is shown.
FIG. 2: the X-ray diffraction pattern spectrum in the example is shown.
FIG. 3: CoN, WN, CrN and Ni prepared in the examples3A mesoporous morphology map of a FeN transmission electron microscope.
FIG. 4: CoN, WN, CrN and Ni prepared in the examples3FeN high resolution transmission electron microscope lattice diagram.
Detailed Description
The present invention will be described in further detail with reference to the following examples, but the present invention is not limited to the following examples.
Examples
1. Preparing a silicon dioxide SBA-15 mesoporous template:
1) 16.5mL of hydrochloric acid (HCl content 12mol/L) was mixed with 112mL of water, 3g of the nonionic triblock copolymer Pluronic P123 was added and the solution was stirred vigorously at 40 ℃ for 3 h;
2) after complete dissolution of P123, 7.427g of tetraethyl orthosilicate was rapidly added to the acidic solution with rapid stirring and kept at 40 ℃ for 24h to obtain a synthetic gel.
3) And then heating the synthesized gel at 90 ℃ for 24h under a static condition, filtering, washing, drying and filtering to obtain a precipitate, and finally calcining at the temperature of more than 500 ℃ to obtain the silica SBA-15 mesoporous template.
2. Preparing cobalt oxide, tungsten oxide, chromium oxide and nickel iron oxide with mesoporous structures:
1) 0.5g of silicon dioxide SBA-15 mesoporous template and 0.8mol/L of metal nitrate solution are weighed as the formerA driver, wherein the cobalt oxide is Co (NO)3)26H2The O and the chromium oxide adopt Cr (NO)3)3·9H2O, tungsten oxide adopt acid hydrate H3[P(W3O10)4]·xH2O), for mixed mesoporous ferronickel oxide, Ni (NO) is adopted3)3·6H2O and Fe (NO)3)3·9H2O is 3: 1; adding the mixed raw materials into 3.6mL of ethanol, stirring for 30min at room temperature, heating to 60 ℃, and evaporating to remove the ethanol to obtain the mesoporous silicon composite material.
2) Putting the mesoporous silicon composite material into a porcelain boat, heating for 4h at 250 ℃ in a muffle furnace, removing the silicon dioxide SBA-15 mesoporous template by using 2mol/L NaOH solution, washing by using deionized water and ethanol, and drying in vacuum at 60 ℃ to respectively prepare cobalt oxide, tungsten oxide, chromium oxide and nickel iron oxide with mesoporous structures.
3. The ordered mesoporous transition metal nitride is prepared according to the following method:
1) loading 10mg of cobalt oxide, tungsten oxide, chromium oxide and nickel iron oxide with mesoporous structures into a pipeline of a programmed heating furnace with a slide rail by using a quartz boat respectively, connecting an ammonia pipeline to the two sections, evacuating the air in the pipeline, filling the air with ammonia, and repeating for 3 times.
2) The furnace is slid to a position where the sample is not affected, the temperature rise is started, and when the temperature reaches the set temperature, the furnace is waited for 10min to be stabilized. The furnace was then pushed towards the sample, with the sample in the center of the heating zone, and the reaction time was recorded until the furnace was pushed away from the sample. The following conditions were used: CoN at 330 deg.C for 15min, WN at 600 deg.C for 10min, 800 deg.C for 30min, CrN at 380 deg.C for Ni3FeN is 30 min.
As shown in fig. 1-4, fig. 1: the X-ray diffraction pattern of the example is shown. FIG. 2: the X-ray diffraction pattern spectrum in the example is shown. FIG. 3: CoN, WN, CrN and Ni prepared in the examples3A mesoporous morphology map of a FeN transmission electron microscope. FIG. 4: CoN, WN, CrN and Ni prepared in the examples3FeN high resolution transmission electron microscope lattice diagram.
As can be seen from fig. 1-4, the transition metal mesoporous nitride prepared by the method has a good pore structure, and both small-angle XRD and TEM images show that the nanopore structure of the transition metal mesoporous nitride is well maintained; the composition of the material is pure phase, and XRD and high-resolution TEM lattice images show that the synthesis of the nitride is successful. These results indicate that the rapid nitridation synthesis method can effectively prepare transition metal nitrides having ordered pore structures.
The above are merely characteristic embodiments of the present invention, and do not limit the scope of the present invention in any way. All technical solutions formed by equivalent exchanges or equivalent substitutions fall within the protection scope of the present invention.
Claims (6)
1. The preparation method of the ordered mesoporous transition metal nitride is characterized by comprising the following steps of: filling transition metal ions in a silicon dioxide SBA-15 mesoporous template, removing the template by using alkali after high-temperature oxidation to generate mesoporous oxide with a mesoporous structure, and then performing high-temperature nitridation treatment on the mesoporous oxide to synthesize the ordered mesoporous transition metal nitride.
2. The method for preparing an ordered mesoporous transition metal nitride according to claim 1, wherein the transition metal ions are one or more of cobalt ions, tungsten ions, chromium ions, nickel ions, and iron ions.
3. The method of preparing an ordered mesoporous transition metal nitride according to claim 1, wherein the mesoporous oxide is one or more of cobalt oxide, tungsten oxide, chromium oxide, and nickel iron oxide.
4. The method for preparing the ordered mesoporous transition metal nitride according to claim 1, wherein the method for preparing the mesoporous template of silicon dioxide SBA-15 comprises:
1) adding a nonionic triblock copolymer Pluronic P123 into hydrochloric acid with the pH value less than 1, and stirring at 30-50 ℃ until the solute is completely dissolved;
2) adding tetraethyl orthosilicate into the solution prepared in the step 1) under the condition of stirring, uniformly mixing and standing for 10-30 h; heating in an oven at 80-90 ℃ for 10-24h under the standing condition, filtering, washing and drying the precipitate obtained by filtering by using deionized water, and finally calcining at the temperature of more than 500 ℃ to obtain the silicon dioxide SBA-15 mesoporous template.
5. The method of preparing an ordered mesoporous transition metal nitride according to claim 1, wherein the method of preparing the mesoporous oxide comprises:
1) adding a silicon dioxide SBA-15 mesoporous template and an oxide precursor into ethanol, uniformly mixing, stirring at room temperature for 30-50min, heating to 60-80 ℃, and evaporating to remove ethanol to obtain a mesoporous silicon composite material;
2) putting the mesoporous silicon composite material into a porcelain boat, heating for 3-4h at the temperature of 250 ℃ in a muffle furnace at 230 ℃, removing the silicon dioxide SBA-15 mesoporous template by using NaOH solution, washing by using deionized water and ethanol, and drying in vacuum at the temperature of 60-80 ℃ to obtain the mesoporous oxide.
6. The method of preparing an ordered mesoporous transition metal nitride according to claim 5, wherein the oxide precursor is a metal salt corresponding to a metal oxide; the metal oxide is one or more of cobalt oxide, chromium oxide, tungsten oxide and nickel iron oxide.
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040096586A1 (en) * | 2002-11-15 | 2004-05-20 | Schulberg Michelle T. | System for deposition of mesoporous materials |
| CN1594073A (en) * | 2004-07-05 | 2005-03-16 | 复旦大学 | Method for preparing low dimensional nanomaterial of metal nitride |
| CN101214928A (en) * | 2008-01-11 | 2008-07-09 | 北京工业大学 | Method for synthesizing high specific surface area ordered mesoporous metal oxide by using hard template agent |
| CN101391753A (en) * | 2008-11-05 | 2009-03-25 | 中国科学院上海硅酸盐研究所 | Method for preparing mesoporous metallic oxide material |
| CN102139920A (en) * | 2010-01-28 | 2011-08-03 | 中国科学院青岛生物能源与过程研究所 | Preparation method for nanoscale transition metal nitride/carbon composite material |
| US20130109895A1 (en) * | 2011-09-23 | 2013-05-02 | Exxonmobil Research And Engineering Company | Low temperature adsorbent for removing sulfur from fuel |
| US10000377B1 (en) * | 2015-10-01 | 2018-06-19 | National Technology & Engineering Solutions Of Sandia, Llc | Nanostructured metal amides and nitrides for hydrogen storage |
| CN108217661A (en) * | 2017-12-26 | 2018-06-29 | 北京化工大学 | A kind of universal method for synthesizing multilevel ordered duct material |
| CN108686688A (en) * | 2017-04-12 | 2018-10-23 | 中国科学院宁波材料技术与工程研究所 | Mesopore surfaces defect Cu-N-TiO2The preparation method of microballoon catalysis material |
| CN109081318A (en) * | 2018-09-06 | 2018-12-25 | 西北工业大学 | A kind of three-dimensional ordered mesoporous cobalt nitride and its preparation method and application |
-
2019
- 2019-08-14 CN CN201910747158.8A patent/CN110586151B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040096586A1 (en) * | 2002-11-15 | 2004-05-20 | Schulberg Michelle T. | System for deposition of mesoporous materials |
| CN1594073A (en) * | 2004-07-05 | 2005-03-16 | 复旦大学 | Method for preparing low dimensional nanomaterial of metal nitride |
| CN101214928A (en) * | 2008-01-11 | 2008-07-09 | 北京工业大学 | Method for synthesizing high specific surface area ordered mesoporous metal oxide by using hard template agent |
| CN101391753A (en) * | 2008-11-05 | 2009-03-25 | 中国科学院上海硅酸盐研究所 | Method for preparing mesoporous metallic oxide material |
| CN102139920A (en) * | 2010-01-28 | 2011-08-03 | 中国科学院青岛生物能源与过程研究所 | Preparation method for nanoscale transition metal nitride/carbon composite material |
| US20130109895A1 (en) * | 2011-09-23 | 2013-05-02 | Exxonmobil Research And Engineering Company | Low temperature adsorbent for removing sulfur from fuel |
| US10000377B1 (en) * | 2015-10-01 | 2018-06-19 | National Technology & Engineering Solutions Of Sandia, Llc | Nanostructured metal amides and nitrides for hydrogen storage |
| CN108686688A (en) * | 2017-04-12 | 2018-10-23 | 中国科学院宁波材料技术与工程研究所 | Mesopore surfaces defect Cu-N-TiO2The preparation method of microballoon catalysis material |
| CN108217661A (en) * | 2017-12-26 | 2018-06-29 | 北京化工大学 | A kind of universal method for synthesizing multilevel ordered duct material |
| CN109081318A (en) * | 2018-09-06 | 2018-12-25 | 西北工业大学 | A kind of three-dimensional ordered mesoporous cobalt nitride and its preparation method and application |
Non-Patent Citations (4)
| Title |
|---|
| SIMON MEYER ET AL.: "Space-confined preparation of high surface area tungsten oxide and tungsten nitride inside the pores of mesoporous silica SBA-15", 《MICROPOROUS AND MESOPOROUS MATERIALS》 * |
| YIFENG SHI ET AL.: "Synthesis of Self-Supported Ordered Mesoporous Cobalt and Chromium Nitrides", 《ADVANCED FUNCTIONAL MATERIALS》 * |
| 姜慧芳、杨明辉: "嵌段共聚物自组装合成Fe2N纳米花", 《中国化学会第30届学术年会摘要集》 * |
| 施益峰: "纳米浇铸法合成有序介孔高温陶瓷材料及金属硫化物、氮化物材料", 《中国博士学位论文全文数据库》 * |
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