CN115072774A - Tetragonal phase layered nitride and low-cost high-efficiency preparation method thereof - Google Patents
Tetragonal phase layered nitride and low-cost high-efficiency preparation method thereof Download PDFInfo
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- CN115072774A CN115072774A CN202210837850.1A CN202210837850A CN115072774A CN 115072774 A CN115072774 A CN 115072774A CN 202210837850 A CN202210837850 A CN 202210837850A CN 115072774 A CN115072774 A CN 115072774A
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- nitride
- bazrn
- sample
- lamellar
- tetragonal phase
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- 150000004767 nitrides Chemical class 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 238000007789 sealing Methods 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 239000010937 tungsten Substances 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- UDEGSYXELBQAAG-UHFFFAOYSA-N azanium;methanol;chloride Chemical compound [NH4+].[Cl-].OC UDEGSYXELBQAAG-UHFFFAOYSA-N 0.000 claims description 2
- 229910052788 barium Inorganic materials 0.000 claims description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 239000004570 mortar (masonry) Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- ZVWKZXLXHLZXLS-UHFFFAOYSA-N zirconium nitride Chemical compound [Zr]#N ZVWKZXLXHLZXLS-UHFFFAOYSA-N 0.000 claims description 2
- -1 zirconium nitride anion Chemical class 0.000 claims description 2
- 238000011049 filling Methods 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 238000005245 sintering Methods 0.000 claims 1
- 229910052726 zirconium Inorganic materials 0.000 claims 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 12
- 239000000463 material Substances 0.000 abstract description 6
- 239000003989 dielectric material Substances 0.000 abstract description 4
- 238000002474 experimental method Methods 0.000 abstract description 4
- 239000000696 magnetic material Substances 0.000 abstract description 4
- 239000011941 photocatalyst Substances 0.000 abstract description 4
- 238000010532 solid phase synthesis reaction Methods 0.000 abstract 2
- 238000007796 conventional method Methods 0.000 abstract 1
- 239000002360 explosive Substances 0.000 abstract 1
- 239000013589 supplement Substances 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 description 7
- 238000003786 synthesis reaction Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000009966 trimming Methods 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/006—Compounds containing, besides zirconium, two or more other elements, with the exception of oxygen or hydrogen
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
Abstract
The invention discloses a method for preparing layered nitride BaZrN by using a high-temperature solid phase method 2 . It is characterized by that its appearance is made into dark red color different from general nitride, and is a tetragonal pyramid structure. The preparation method has the advantages of simple related composition and preparation process, short period, and capability of being obtained only by two times of high-temperature solid-phase synthesis, and greatly shortens the time consumption compared with the conventional method. And the cost is low, one of expensive raw materials required by experiments is-Ba 3 N 2 Can be obtained in the experimental process. And the dangerous high NaN is avoided in the experiment 3 The (explosive) nitrogen source is used as a nitrogen source supplement mode, so that the experimental safety is greatly improved. The invention can be widely used in the fields of fluorescent materials, photocatalysts, dielectric materials, magnetic materials and the like.
Description
Technical Field
The invention relates to a layered nitride material and a preparation method thereof in the fields of fluorescent materials, photocatalysts, dielectric materials, magnetic materials and the like.
Background
Oxygen and nitrogen have close chemical structures and electronic characteristics, such as polarizability, electronegativity, coordination number, and ionic radius, and form similar structural types when combined with cations and displace each other at the same sites to form solid solutions. Nitrides are therefore a very important and yet to be further explored system in the search for new substances and materials. Nitrogen has a larger effective charge, ion size, polarizability, coordination number and lower electronegativity than oxygen, giving it more freedom and diversity in the structural framework than oxides. The introduction of nitrogen can adjust the width of a forbidden band, so that the absorption of different wave bands of light of the sample is changed, and different colors are presented. The pigment containing heavy metals can be replaced by the pigment, so that the harm of the heavy metals to people and nature is reduced. Thus, C 3 N 4 、GaN、CaTiN 2 、Mo 2 Nitrides such as N have been produced, so that the nitrides have unusual performances and great potentials in the aspects of photocatalysts, dielectric materials, magnetic materials, lithium ion batteries, catalytic materials and the like. However, the nitride preparation conditions are harsh, and the samples are unstable, so that the research progress of people on the nitride is slow. Such as BaZrN 2 In the conventional synthesis, NaN was used in the previous experiment 3 As the nitrogen source, the risk of the experiment was greatly increased, and Ba was used 3 N 2 The synthesis cost is extremely high as a raw material for synthesis, and the synthesis in multiple steps increases the synthesis time and reduces the synthesis efficiency.
Disclosure of Invention
The low-cost and high-efficiency preparation steps of the tetragonal phase layered nitride are as follows:
(1) the raw material metal barium particles are evenly and loosely placed in a tungsten crucible, and a sealing film is used for sealing. Putting the mixture into a tube furnace, introducing ammonia gas, heating to 600 ℃ and ammoniating for 6 hours
(2) The aminated sample and zirconium nitride powder were mixed and ground in an agate mortar at a ratio of 0.68:1 for about 40 minutes, and the ground powder was again charged into a tungsten crucible and sealed.
(3) The sample was placed in a tube furnace and 5% N was passed 2 /H 2 The mixed gas is heated to 1200 ℃ and sintered for 12 hours.
(4) Taking out and grinding the sample, and cleaning the sample by using an ammonium chloride-methanol solution to obtain the required target tetragonal phase lamellar nitride-BaZrN 2 。
The tetragonal phase lamellar nitride BaZrN prepared by the invention 2 The preparation method has the advantages of simple preparation process, greatly reduced preparation time, high experimental safety, no high-temperature operation, replacement of expensive compounds by low-cost substances, and greatly reduced preparation cost. Provides a thought for the preparation and synthesis of related nitrides.
Drawings
FIG. 1 shows BaZrN 2 Powder X-ray diffraction fine trimming map
Detailed Description
The preparation method is as described above, phase analysis is carried out on the sintered sample by the powder X-ray diffraction method, figure 1 is a refined graph of the X-ray diffraction graph, and the result after the refinement shows that the single tetragonal layered nitride BaZrN is obtained 2 。
The invention can be widely used in the fields of fluorescent materials, photocatalysts, dielectric materials, magnetic materials and the like.
Claims (2)
1. KCoO crystallized in tetragonal space group P4/nmm 2 Lamellar nitride-BaZrN 2 Characterized in that it has a dark red appearance different from that of general nitrides and has a structure in which Zr atom is the center of symmetry and has a two-dimensionally linked zirconium nitride anion [ ZrNN 4/4 ] 2- And Ba at the top 2+ The edges of the bottom of each pyramid are shared, and the tops of the pyramid are arranged in a staggered mode.
2. KCoO crystallized in tetragonal space group P4/nmm according to claim 1 2 Lamellar nitride-BaZrN 2 The method is characterized in that the low-cost and high-efficiency preparation steps of the tetragonal phase layered nitride are as follows:
(1) uniformly and loosely placing raw material metal barium particles in a tungsten crucible, and sealing with a sealing film; putting the mixture into a tubular furnace, introducing ammonia gas, heating to 600 ℃ and ammoniating for 6 hours;
(2) mixing and grinding the sample obtained by ammoniation and zirconium nitride powder in an agate mortar according to the ratio of 0.68:1 for about 40 minutes, and filling the ground powder into a tungsten crucible again and sealing;
(3) the sample was placed in a tube furnace and 5% N was passed 2 /H 2 Heating the mixed gas to 1200 ℃ and sintering for 12 hours;
(4) taking out and grinding the sample, and cleaning the sample by using an ammonium chloride-methanol solution to obtain the required target tetragonal phase lamellar nitride-BaZrN 2 。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210837850.1A CN115072774A (en) | 2022-07-16 | 2022-07-16 | Tetragonal phase layered nitride and low-cost high-efficiency preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210837850.1A CN115072774A (en) | 2022-07-16 | 2022-07-16 | Tetragonal phase layered nitride and low-cost high-efficiency preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115072774A true CN115072774A (en) | 2022-09-20 |
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|---|---|---|---|
| CN202210837850.1A Pending CN115072774A (en) | 2022-07-16 | 2022-07-16 | Tetragonal phase layered nitride and low-cost high-efficiency preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100297505A1 (en) * | 2009-05-21 | 2010-11-25 | Toyota Jidosha Kabushiki Kaisha | Method of producing nitrided li-ti compound oxide, nitrided li-ti compound oxide, and lithium-ion battery |
| CN103878011A (en) * | 2014-04-17 | 2014-06-25 | 哈尔滨工业大学 | Method for synthesizing GaN: ZnO solid solution photocatalyst |
| CN107983387A (en) * | 2017-12-05 | 2018-05-04 | 福州大学 | A kind of preparation method of carbonitride/selenic acid bismuth composite material and application |
-
2022
- 2022-07-16 CN CN202210837850.1A patent/CN115072774A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100297505A1 (en) * | 2009-05-21 | 2010-11-25 | Toyota Jidosha Kabushiki Kaisha | Method of producing nitrided li-ti compound oxide, nitrided li-ti compound oxide, and lithium-ion battery |
| CN103878011A (en) * | 2014-04-17 | 2014-06-25 | 哈尔滨工业大学 | Method for synthesizing GaN: ZnO solid solution photocatalyst |
| CN107983387A (en) * | 2017-12-05 | 2018-05-04 | 福州大学 | A kind of preparation method of carbonitride/selenic acid bismuth composite material and application |
Non-Patent Citations (2)
| Title |
|---|
| AKIHIRO SHIRAISHI ET AL.: "Design, Synthesis, and Optoelectronic Properties of the High-Purity Phase in Layered AETMN2 (AE = Sr, Ba; TM = Ti, Zr, Hf) Semiconductors", INORGANIC CHEMISTRY * |
| XIAOHUI LI ET AL.: "High-Dielectric-Permittivity Layered Nitride CaTiN2", CHEMISTRY OF MATERIALS * |
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