CN102259935B - A surfactant-assisted hydrothermal method for the preparation of bird's nest-shaped Co3O4 - Google Patents
A surfactant-assisted hydrothermal method for the preparation of bird's nest-shaped Co3O4 Download PDFInfo
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- 238000001027 hydrothermal synthesis Methods 0.000 title abstract description 8
- 239000004094 surface-active agent Substances 0.000 title abstract 2
- 238000002360 preparation method Methods 0.000 title description 8
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 title description 3
- 239000007864 aqueous solution Substances 0.000 abstract description 6
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 abstract description 6
- 229910021645 metal ion Inorganic materials 0.000 abstract description 5
- 229910001220 stainless steel Inorganic materials 0.000 abstract description 5
- 239000010935 stainless steel Substances 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 3
- 239000008204 material by function Substances 0.000 abstract description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 abstract 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 229910020599 Co 3 O 4 Inorganic materials 0.000 abstract 1
- 244000000626 Daucus carota Species 0.000 abstract 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 abstract 1
- 235000011114 ammonium hydroxide Nutrition 0.000 abstract 1
- 235000005770 birds nest Nutrition 0.000 abstract 1
- -1 polytetrafluoroethylene Polymers 0.000 abstract 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 abstract 1
- 239000004810 polytetrafluoroethylene Substances 0.000 abstract 1
- 239000002244 precipitate Substances 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- 235000005765 wild carrot Nutrition 0.000 abstract 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 8
- 239000013543 active substance Substances 0.000 description 7
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical compound CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 230000005291 magnetic effect Effects 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000013019 agitation Methods 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 238000011068 loading method Methods 0.000 description 4
- 238000000967 suction filtration Methods 0.000 description 4
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 4
- 238000010792 warming Methods 0.000 description 4
- 206010013786 Dry skin Diseases 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 229910052596 spinel Inorganic materials 0.000 description 3
- 239000011029 spinel Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 239000002071 nanotube Substances 0.000 description 2
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- ASKVAEGIVYSGNY-UHFFFAOYSA-L cobalt(ii) hydroxide Chemical compound [OH-].[OH-].[Co+2] ASKVAEGIVYSGNY-UHFFFAOYSA-L 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
一种制备鸟巢形Co3O4的表面活性剂辅助的水热方法，属于功能材料技术领域。包括以下步骤：在搅拌条件下，将氨水溶滴加到浓度为0.33-0.34mol/LCo(NO3)2的水溶液中，控制其pH值9～10，使金属离子完全沉淀，加入乙二胺(与Co(NO3)2的摩尔比2∶3)或十二胺(与Co(NO3)2的摩尔比43∶100)，转移至内衬为50mL聚四氟乙烯的不锈钢反应釜中，体积填充量80％，于120℃恒温24h，或于140℃或200℃恒温12h，冷却至室温，抽滤、洗涤、60℃干燥12h、研磨，在空气中以1℃/min的速率升温至300℃并保持4h。样品为表面具有层状的鸟巢状结构。A surfactant-assisted hydrothermal method for preparing bird's nest-shaped Co 3 O 4 belongs to the technical field of functional materials. The method includes the following steps: under the condition of stirring, add ammonia solution dropwise to the aqueous solution with a concentration of 0.33-0.34mol/LCo(NO 3 ) 2 , control its pH value to 9-10 to completely precipitate metal ions, and add ethylenediamine (2:3 molar ratio to Co(NO 3 ) 2 ) or dodecylamine (43:100 molar ratio to Co(NO 3 ) 2 ), transferred to a stainless steel reactor lined with 50 mL polytetrafluoroethylene , with a volume filling of 80%, keep the temperature at 120°C for 24 hours, or at 140°C or 200°C for 12 hours, cool to room temperature, filter, wash, dry at 60°C for 12 hours, grind, and heat up at a rate of 1°C/min in the air to 300°C and keep for 4h. The sample has a layered bird's nest structure on the surface.
Description
Technical field
The present invention relates to a kind of special appearance Co that has
3O
4The preparation method, relate to specifically and adopt the Co that has bird-nest-shaped take quadrol or amino dodecane as the hydrothermal method preparation of tensio-active agent
3O
4, belong to technical field of function materials.
Background technology
Co
3O
4Be a kind of important functional materials, be widely used in the fields such as electrochromic device, beramic color, catalysis, solid state sensor, magnetics, solar energy absorption plant and energy storage (intercalation compound of Li-Ion rechargeable battery).Therefore, to Co
3O
4The research work of synthetic method a lot.People have synthesized the Co of various patterns
3O
4, the nanometer ball of hollow (S.A.Makhlouf, J.Magn.Mater. for example, 2002,246:184-190), fibrous (B.B.Lakshmi, et al., Chem.Mater., 1997,9:2544-2550), nanometer rod, nanotube, nano-structure film (A.Gulino, et al., Chem.Mater., 2003,15:3748-3752) etc.The Co of nanometer wire
3O
4Can pass through porous Al
2O
3Or virus (K.T.Nam, et al., Science, 2006,312:885-888) prepare for template.Can obtain Co by the heating cobaltous hydroxide
3O
4Nanometer rod (E.Hosono, et al., J.Mater.Chem., 2005,15:1938-1945).Adopt the method for not adding tensio-active agent, by prepare the nano wire of hollow in different matrix (such as transparent conducting glass, silicon wafer, Copper Foil etc.).
Ren etc. (L.Ren, et al., Chem.Phys.Lett., 2009,476:78-83) take cetyl trimethylammonium bromide (CTAB) as tensio-active agent, through having prepared the cobaltosic oxide nano rod after hydrothermal treatment consists and the roasting.Jiang etc. (J.Jiang, et al., J.Phys.Chem.C, 2010,114:929-932) employing is not added the hydrothermal method of tensio-active agent and has been prepared cobalt oxide porous nano line through the roasting precursor.Zhuo etc. (L.H.Zhuo, et al., Cryst.Growth Des., 2009,9:1-6) mixing solutions take water and methyl alcohol has prepared Co as the alcohol-hydrothermal method of solvent and through the roasting precursor
3O
4Nanotube.The present invention reports that adopting quadrol or amino dodecane is the Co that the hydrothermal method preparation of tensio-active agent has bird-nest-shaped
3O
4Up to now, relevant bird-nest-shaped Co
3O
4The background technology of preparation aspect there is no bibliographical information.
Summary of the invention
The object of the present invention is to provide the auxiliary hydrothermal method preparation of a kind of tensio-active agent to have the Co of bird-nest-shaped
3O
4Novel method.
Preparation provided by the invention has bird-nest-shaped Co
3O
4The preparation method be under agitation condition, ammonia soln to be added drop-wise to contain Co (NO
3)
2Transparent aqueous solution in, Co (NO
3)
2The concentration of the aqueous solution is 0.33～0.34mol/L, controls its pH value between 9～10, and metal ion is precipitated fully.Then add a certain amount of quadrol or amino dodecane, quadrol and Co (NO
3)
2Mol ratio be 2: 3, amino dodecane and Co (NO
3)
2Mol ratio be 43: 100, again it is transferred in the stainless steel cauldron that liner is the 50mL tetrafluoroethylene, volume loading level 80%, put into thermostat container in 120 ℃ of constant temperature 24h, or put into thermostat container in 140 ℃ or 200 ℃ of constant temperature 12h, to be cooled to room temperature, with the turbid solution suction filtration that obtains, solids wash, 60 ℃ of dry 12h, grind after, in air atmosphere, be warming up to 300 ℃ and keep 4h at 300 ℃ with the speed of 1 ℃/min again, obtain bird-nest-shaped Co
3O
4Black powder.
Gained black powder product is characterized with technology such as X-ray diffraction (XRD) instrument, high resolution scanning electron microscopes (HRSEM), and sample is the nest like structure that the surface has laminate structure, and it is the Co of pure phase as can be known by the XRD test
3O
4The Co of nest like structure
3O
4Has important use at aspects such as electrochromic device, beramic color, catalysis, solid state sensor, magnetics, solar energy absorption plant and energy storage.
Description of drawings
Fig. 1 is Co
3O
4XRD spectra
Wherein curve (a) is embodiment 1, and curve (b) is embodiment 2, and curve (c) is embodiment 3;
Fig. 2 is Co
3O
4The HRSEM photo
Wherein (a) is embodiment 1, (b) is embodiment 2, and curve (c) is embodiment 3.
Embodiment
Be further to understand the present invention, the below elaborates with embodiment, and provides accompanying drawing and describe the bird-nest-shaped Co that the present invention obtains
3O
4, but the invention is not restricted to following examples.
Embodiment 1: under the magnetic agitation condition, ammonia soln slowly is added drop-wise to contains 10mmol Co (NO
3)
2The transparent aqueous solution of 30mL in, control its pH value between 9～10, metal ion is precipitated fully.The quadrol that adds again 1mL, then mixed solution is transferred to (80% volume loading level) in the stainless steel cauldron that the 50mL liner is tetrafluoroethylene, put into again thermostat container in 140 ℃ of insulation 12h, afterwards at room temperature cooling, with (60 ℃ of the turbid solution suction filtration, washing, the dryings that obtain, 12h), grind evenly, obtain the target product precursor, again it is placed retort furnace to be warming up to 300 ℃ and keep 4h at 300 ℃ at air atmosphere with the speed of 1 ℃/min, namely get single-phase cubic spinel type Co
3O
4Powder, pattern are the bird-nest-shaped that has more uniformly the scale surface, and diameter is about 36 μ m, and its XRD spectra is seen Fig. 1 (a), and the HRSEM photo is seen Fig. 2 (a).
Embodiment 2: under the magnetic agitation condition, ammonia soln slowly is added drop-wise to contains 10mmol Co (NO
3)
2The transparent aqueous solution of 30mL in, control its pH value between 9～10, metal ion is precipitated fully.The amino dodecane that adds again 1mL, then it is transferred to (80% volume loading level) in the stainless steel cauldron that the 50mL liner is tetrafluoroethylene, put into again in the thermostat container in 120 ℃ of insulation 24h, afterwards at room temperature cooling, with (60 ℃ of the turbid solution suction filtration, washing, the dryings that obtain, 12h), grinding evenly obtains the target product presoma, place retort furnace to be warming up to 300 ℃ and at 300 ℃ of lower 4h of maintenance at air atmosphere with the speed of 1 ℃/min, namely get single-phase cubic spinel type Co
3O
4Powder, pattern are more uniform ganoid bird-nest-shaped, and diameter is about 42 μ m, and its XRD spectra is seen Fig. 1 (b), and the HRSEM photo is seen Fig. 2 (b).
Embodiment 3: under the magnetic agitation condition, ammonia soln slowly is added drop-wise to contains 10mmol Co (NO
3)
2The transparent aqueous solution of 30mL in, control its pH value between 9～10, metal ion is precipitated fully.The quadrol that adds again 1mL, then it is transferred to (80% volume loading level) in the stainless steel cauldron that the 50mL liner is tetrafluoroethylene, put into again in the thermostat container in 200 ℃ of insulation 12h, afterwards at room temperature cooling, with (60 ℃ of the turbid solution suction filtration, washing, the dryings that obtain, 12h), grinding evenly obtains the target product presoma, place retort furnace to be warming up to 300 ℃ and at 300 ℃ of lower 4h of maintenance at air atmosphere with the speed of 1 ℃/min, namely get single-phase cubic spinel type Co
3O
4Powder, pattern are the bird-nest-shaped with scale surface, and diameter is about 30 μ m, and its XRD spectra is seen Fig. 1 (c), and the HRSEM photo is seen Fig. 2 (c).
Claims (3)
1. one kind prepares bird-nest-shaped Co
3O
4The auxiliary hydrothermal method of tensio-active agent, it is characterized in that, may further comprise the steps: under the magnetic agitation condition, ammonia soln slowly is added drop-wise to contains 10mmolCo (NO
3)
2The transparent aqueous solution of 30mL in, control its pH value between 9 ~ 10, metal ion is precipitated fully; The quadrol that adds again 1mL, then mixed solution is transferred in the stainless steel cauldron that the 50mL liner is tetrafluoroethylene, making the volume loading level is 80%, put into again thermostat container in 140 ℃ of insulation 12h, afterwards at room temperature cooling with the turbid solution suction filtration that obtains, washing, 60 ℃ of dry 12h, grind evenly, obtains the target product precursor, again it is placed retort furnace to be warming up to 300 ℃ and keep 4h at 300 ℃ at air atmosphere with the speed of 1 ℃/min, namely get single-phase cubic spinel type Co
3O
4Powder.
2. one kind prepares bird-nest-shaped Co
3O
4The auxiliary hydrothermal method of tensio-active agent, it is characterized in that, may further comprise the steps: under the magnetic agitation condition, ammonia soln slowly is added drop-wise to contains 10mmolCo (NO
3)
2The transparent aqueous solution of 30mL in, control its pH value between 9 ~ 10, metal ion is precipitated fully, the amino dodecane that adds again 1mL, then it is transferred in the stainless steel cauldron that the 50mL liner is tetrafluoroethylene, make volume loading level 80%, put into again in the thermostat container in 120 ℃ of insulation 24h, afterwards at room temperature cooling, with the turbid solution suction filtration that obtains, washing, 60 ℃ of dry 12h, grind and evenly obtain the target product presoma, place retort furnace to be warming up to 300 ℃ and at 300 ℃ of lower 4h of maintenance at air atmosphere with the speed of 1 ℃/min, namely get single-phase cubic spinel type Co
3O
4Powder.
3. one kind prepares bird-nest-shaped Co
3O
4The auxiliary hydrothermal method of tensio-active agent, it is characterized in that, may further comprise the steps: under the magnetic agitation condition, ammonia soln slowly is added drop-wise to contains 10mmolCo (NO
3)
2The transparent aqueous solution of 30mL in, control its pH value between 9 ~ 10, metal ion is precipitated fully, the quadrol that adds again 1mL, then it is transferred in the stainless steel cauldron that the 50mL liner is tetrafluoroethylene, make volume loading level 80%, put into again in the thermostat container in 200 ℃ of insulation 12h, afterwards at room temperature cooling, with the turbid solution suction filtration that obtains, washing, 60 ℃ of dry 12h, grind and evenly obtain the target product presoma, place retort furnace to be warming up to 300 ℃ and at 300 ℃ of lower 4h of maintenance at air atmosphere with the speed of 1 ℃/min, namely get single-phase cubic spinel type Co
3O
4Powder.
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| CN102674482A (en) * | 2012-05-22 | 2012-09-19 | 上海大学 | Dendriform cobalt oxide nano material and preparation method thereof |
| CN106268814A (en) * | 2015-05-20 | 2017-01-04 | 中国科学院大连化学物理研究所 | A kind of flower-shaped Cobalto-cobaltic oxide catalyst and its preparation method and application |
| CN106180748B (en) * | 2016-07-15 | 2018-04-03 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of preparation method for carrying the porous cobaltosic oxide nano composite material of silver |
| CN107367527A (en) * | 2017-06-29 | 2017-11-21 | 滨州学院 | It is a kind of that there is highly sensitive spindle zinc oxide gas sensitive to triethylamine |
| CN109422295B (en) * | 2017-09-05 | 2021-09-17 | 中国科学院大连化学物理研究所 | Preparation method of sea urchin-shaped cobaltosic oxide material |
| CN114105218A (en) * | 2021-11-30 | 2022-03-01 | 泉州市云箭测控与感知技术创新研究院 | Preparation method of bird nest-shaped cobaltosic oxide material |
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| 孙灵娜.水热法合成四氧化三钴纳米材料.《材料科学与工程学报》.2011,第29卷(第1期),第18页左栏第4-5段至第18页右栏第1行. |
| 水热法合成四氧化三钴纳米材料;孙灵娜;《材料科学与工程学报》;20110228;第29卷(第1期);第18页左栏第4-5段至第18页右栏第1行 * |
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