CN109461557A - Orderly inorganic-organic hybrid functional nano-materials and its preparation with room-temperature ferromagnetic - Google Patents
Orderly inorganic-organic hybrid functional nano-materials and its preparation with room-temperature ferromagnetic Download PDFInfo
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Abstract
The object of the present invention is to provide a kind of orderly inorganic-organic hybrid functional nano-materials and preparation method thereof with room-temperature ferromagnetic, it is prepared using chemical liquid phase reaction, the inorganic-organic hybrid functional nano-materials have two-dimensional nano piece or Nanoparticulate microstructure, and inorganic structure unit is the β-Fe with tetragonal structure3‑ xMxSe4‑yQy, wherein M=Cr, Co；Q=S, Te；0≤x<3；0≤y < 4, organic structure ele are metal organo-amine complex.The magnetic order temperature of gained inorganic-organic hybrid functional nano-materials is higher than room temperature, and there is periodic structure, this method preparation manipulation is simple, raw material is easily obtained, short preparation period, temperature are low, it can be used for synthesizing having a size of 500 nanometers -6 microns, graininess hybrid nano-material of the thickness in 100-300 nanometers of sheet hybrid nano-material or 50-500 nanometer.
Description
Technical field
The invention belongs to magnetic organic functions field of nanometer material technology, and in particular to a kind of magnetic order temperature is higher than the tool of room temperature
There are the inorganic-organic hybrid functional nano-materials and preparation method thereof of periodic arrangement.
Background technique
Different from phase domain scale come the inorganic-organic nanocomposite that defines, " Inorganic-Organic Hybrid Material " be by
The uniform heterogeneous material of a kind of chemical component that organic phase and inorganic phase are constituted.According to different preparation methods can by it is inorganic-
Organic hybrid nano material is divided into: (1) organic phase is embedded in inorganic network；(2) inorganic phase is embedded in organic network；(3)
Organic phase-inorganic phase forms inierpeneirating network structure；(4) cross-linked structure is formed by covalent bond.For magnetic inorganic-organic hybrid
Nano material is obtained with organic phase by above-mentioned hybrid form if magnetic inorganic has mutually formed nanostructure
Hybrid material is difficult the magnetic property for occurring different from inorganic nano material itself.By preparation method from bottom to top, directly molten
So that metal ion or atom is grown to magnetic alloy sub-nanometer structure (thickness is in several unit cell sizes) in liquid, then is crosslinked with valence link
Effect makes organic molecule and inorganic structure unit (one-dimensional chain, two-dimensional layer, three-dimensional segment etc.) generate periodic arrangement, is formed new
Hybrid material with periodic arrangement will likely show the magnetic property (change of such as Curie temperature) different from inorganic phase.Stratiform
Inorganic-organic hybrid functional nano-materials with periodic arrangement combine inorganic (Asia) nanometer sheet material, organic molecule and nanometer
The good characteristic of material not only makes the physical property such as the light, electricity, thermal and magnetic of material that huge change occur, and also possesses low-density, multi-functional
Etc. advantages.
II-VI group has the inorganic-organic hybridization semiconductor of periodic arrangement, changes MQ (M=in very narrow range
Mn,Zn,Cd；Q=S, Se, Te) sub-nanometer structure size, regulate and control inorganic-organic hybridization semiconductor material with can be convenient
(MQ)LxBand gap (Eg), wherein L be organic amine or hydrazine [X.Y.Huang, J.Li, J.Am.Chem.Soc.129 (2007)
3157.].Inorganic-Organic Hybrid Material GeOxThe Central Asia /en (en: ethylenediamine) nano periodic structure leads to strong quantum effect
[O.S.Gao,Y.Tang.Adv.Mater.20(2008)1837.]。[Fe(en)3]2[Fe16S20]enH2Stratiform Hybrid semiconductor,
Along structure cell c-axis direction occur zero or close to zero thermal expansion special nature [M.Wu, J.Li, Chem.Commun.46
(2010)1649.].Sunyang etc. finds organic metal framework structure (MOF) [(CH3)2NH2]Fe(HCOO)3In there are magnon tunnels
Wear phenomenon [Y.Tian, et al.Phys.Rev.Lett.112 (2014) 017202.] and [(CH3)2NH2]Cu(HCOO)3In
Multiferroic and magneto-electric coupled phenomenon [Y.Tian, et al.Phys.Status Solidi RRL 9 (2015) 62.].Han etc.
Antiferromagnetic perovskite-like (the C of preparation2H5NH3)2[FeIICl4] stratiform hybrid material, 380K to 10K temperature range experienced from
The orthogonal differentiation [J.Han, et al.Inorg.Chem.54 (2015) 2866.] for arriving monocline again is arrived in four directions.In no magnetism
The metal-organic framework of ion, discovery are based on the length of antiferromagnetic Cu (II) dimer structure unit and non magnetic organic molecule
Journey ferromagnetic ordering [L.Shen, et al.J.Am.Chem.Soc.134 (2012) 17286.].Mixing using organic amine and water is molten
Agent, with solvent thermal process, Yu Shuhong etc. is prepared for [Fe18S25](TETAH)14Nanobelt [Z.A.Zang, et
Al.Chem.Mater.20 (2008) 4749-4755.] and CoSe2- amine (protonated) nanobelt [M.R.Gao, et
al.J.Am.Chem.Soc.131(2009)7486.].In the past the Inorganic-Organic Hybrid Material with periodic arrangement of preparation
Magnetic order temperature be typically well below room temperature (200K or less), how by the Inorganic-Organic Hybrid Material with periodic arrangement
Magnetic order temperature to be increased to room temperature or more be a problem.
The present invention uses chemical liquid phase reaction, using metal organo-amine complex as organic structure ele, tetragonal structure iron
Chalcogenide is inorganic structure unit, and it is miscellaneous to have synthesized the inorganic-organic with periodic arrangement with room temperature magnetism for the first time
Change nano material.It is this to be received by inorganic-organic hybridization with periodic arrangement of the chemical solution preparation with room temperature magnetism
The method of rice material is not reported.
Summary of the invention
The object of the present invention is to provide a kind of orderly inorganic-organic hybrid functional nano-materials and its system with room-temperature ferromagnetic
Preparation Method is received using the inorganic-organic hybridization with periodic structure that chemical liquid phase reaction preparation magnetic order temperature is higher than room temperature
Rice material, this method preparation manipulation is simple, raw material is easily obtained, and short preparation period, temperature are low, can be used for synthesizing having a size of
500 nanometers -6 microns, thickness is received in the graininess hydridization of 100-300 nanometers of sheet hybrid nano-material or 50-500 nanometer
Rice material.
Technical solution of the present invention is as follows:
A kind of orderly inorganic-organic hybrid functional nano-materials with room-temperature ferromagnetic, it is characterised in that: use chemical liquid phase
Method preparation, the inorganic-organic hybrid functional nano-materials have two-dimensional nano sheet microstructure, micro- having a size of 500 nanometer -6
Rice, thickness is at 100-300 nanometers；Or there is Nanoparticulate microstructure, size is at 50-500 nanometers.The nano material
Inorganic structure unit be the β-Fe with tetragonal structure3-xMxSe4-yQy, wherein M=Cr, Co；Q=S, Te；0≤x<3；0
≤ y < 4, organic structure ele are metal organo-amine complex.
Orderly inorganic-organic hybrid functional nano-materials of the present invention with room-temperature ferromagnetic, it is characterised in that: the nothing
Machine-organic hybrid nano material has the ferrimagnetism energy of room temperature, and the crystal structure with periodic arrangement.
The present invention also provides the preparation sides of the orderly inorganic-organic hybrid functional nano-materials with room-temperature ferromagnetic
Method, which is characterized in that prepared using chemical liquid phase reaction, the specific steps are as follows:
(1) raw material are mixed with organic amine, is placed in 250 milliliters -2000 milliliters (ml) four-hole boiling flasks and is allowed to dissolve, obtains
To uniform precursor solution；Air is excluded using inert gas, under magnetic stirring, is warming up to 120-200 DEG C, 0-120 points of heat preservation
Clock；Precursor solution is warming up to reaction temperature again, keeps the temperature 0.5 hour to 24 hours in the reaction temperature, it after reaction, will
Reaction system is down to room temperature；
(2) it is centrifugated reaction product solution, supernatant is abandoned, obtains precipitated product；
(3) it (is preferably washed 3 times) after being washed with dehydrated alcohol, is dried in a vacuum, obtains powder product.
Wherein, before step (1) described raw material include the metal precursor and selenium for being dissolvable in water organic amine, sulphur or tellurium
Drive body.
In the metal precursor, the raw material of iron are one of ferric acetyl acetonade, acetylacetone,2,4-pentanedione ferrous iron (preferably second
Acyl acetone iron), the raw material further include the presoma of the cobalt for being dissolvable in water organic solvent, chromium, nickel and/or manganese, wherein cobalt
Presoma is acetylacetone cobalt, and the presoma of chromium is chromium acetylacetonate, and the presoma of nickel is nickel acetylacetonate, and the presoma of manganese is
Manganese acetylacetonate.
The presoma (chalcogen raw material) of the selenium, sulphur or tellurium is selenium powder, titanium dioxide selenium powder (preferably selenium dioxide
Powder)；One of sodium selenide, vulcanized sodium, telluride sodium are a variety of.
The molar ratio of metallic atom and chalcogen atom is between 1:1 to 1:2 in step (1).
Organic solvent described in step (1) is the organic amine solvent with reproducibility, preferably diethylenetriamine, triethylene
Tetramine (triethylenetetramine, TETA), tetraethylenepentamine (tetraethylenepentamine, TEPA) He Wuyi
In alkene hexamine one or more (most preferably tetraethylenepentamine).
Raw material usage described in step (1) is 0.05mmol-120mmol, organic solvent 20-1000ml.
Reaction temperature described in step (1) is 180-300 DEG C.
The present invention has the orderly inorganic-organic hybrid functional nano-materials of room-temperature ferromagnetic using chemical liquid phase reaction preparation, excellent
Point is: process is simple, it is low in cost, need not reagent and equipment expensive or that have particular/special requirement, obtain with room temperature ferromagnetic
The inorganic-organic hybrid functional nano-materials of property.
Detailed description of the invention
Fig. 1 is the Inorganic-Organic Hybrid Material (β-Fe with periodic structure3Se4)4The x- ray of [Fe (TEPA)] spreads out
Penetrate figure；
Fig. 2 is Inorganic-Organic Hybrid Material (β-Fe3Se4)4Scanning electron microscope (SEM) photo of [Fe (TEPA)]；
Fig. 3 is Inorganic-Organic Hybrid Material (β-Fe3Se4)4Transmission electron microscope (TEM) photo of [Fe (TEPA)]；
Fig. 4 is Inorganic-Organic Hybrid Material (β-Fe3Se4)4The thermal gravimetric analysis curve of [Fe (TEPA)] is higher than 530K hydridization
Material thermally decomposes；
Fig. 5 is Inorganic-Organic Hybrid Material (β-Fe3Se4)4Magnetic hysteresis when (a) 300K and (b) 5K of [Fe (TEPA)] is returned
Line；
Fig. 6 is the Inorganic-Organic Hybrid Material (β-Fe being heat-treated at 500K3Se4)4(a) 300K of [Fe (TEPA)] and
(b) hysteresis loop when 5K；
Fig. 7 is the Inorganic-Organic Hybrid Material (β-Fe with periodic structure3Se4)4[Fe(TETA)4/3] x- ray
Diffraction pattern；
Fig. 8 is Inorganic-Organic Hybrid Material (β-Fe3Se4)4The hysteresis loop of (a) 300K and (b) 5K of [Fe (TETA)]；
Fig. 9 is Inorganic-Organic Hybrid Material (β-Fe2.5Cr0.5Se4)4The X-ray diffraction figure of [Fe (TEPA)].
Specific embodiment
Following embodiment will be further described the present invention, but not thereby limiting the invention.
Embodiment 1
Ferric acetyl acetonade (5.25mmol) and selenium dioxide (6mmol) are dissolved in tetraethylenepentamine (TEPA, 60ml), and
It is placed in four-hole boiling flask, after leading to high pure nitrogen exclusion air, under magnetic stirring, mixed solution is warming up to 180 DEG C, heat preservation 0.5
Hour；Mixed solution is warming up to 280 DEG C again, keeps the temperature 3 hours, obtains inorganic-organic hybrid functional nano-materials (β-Fe3Se4)4[Fe
(TEPA)].It is cooled to room temperature, by (β-Fe3Se4)4The centrifuge separation of [Fe (TEPA)] nano material, and 3 are washed with dehydrated alcohol
Time, it is dried in a vacuum, and be saved in vacuum.
The crystal structure of product is determined using X-ray diffraction, it is determined that object is mutually the (β-of tetragonal structure
Fe3Se4)4[Fe (TEPA)], as shown in Figure 1.Its scanning electron microscope (SEM) photo shows (β-Fe3Se4)4[Fe (TEPA)] nanometer
The size of piece is 500 nanometers -5 microns, and thickness is at 100-300 nanometers, as shown in Figure 2.(β-Fe3Se4) [Fe (TEPA)] nanometer sheet
Transmission electron microscope (TEM) photo it is as shown in Figure 3.(β-Fe3Se4) [Fe (TEPA)] nanometer sheet thermal gravimetric analysis curve, measurement shows
Temperature is higher than 530K hybrid material and thermally decomposes, as shown in Figure 4.As-deposited state Inorganic-Organic Hybrid Material (β-Fe3Se4)4[Fe
(TEPA)] (a) 300K (Kelvin) and low temperature (b) 5K hysteresis loop of nanometer sheet, as shown in Figure 5.It is heat-treated when at 500K
Inorganic-Organic Hybrid Material (β-Fe3Se4)4[Fe (TEPA)], heat treated hybrid material magnetism is remarkably reinforced, as Fig. 6 gives
Hysteresis loop when (a) 300K and (b) 5K out.
Embodiment 2
Ferric acetyl acetonade (5.25mmol) and selenium dioxide (6mmol) are dissolved in triethylene tetramine (TETA, 60ml), and
It is placed in four-hole boiling flask, after leading to high pure nitrogen exclusion air, under magnetic stirring, mixed solution is warming up to 180 DEG C, heat preservation 0.5
Hour；Mixed solution is warming up to 250 DEG C again, keeps the temperature 3 hours, obtains inorganic-organic hybrid functional nano-materials (β-Fe3Se4)4[Fe
(TETA)4/3].It is cooled to room temperature, by (β-Fe3Se4)4[Fe(TETA)4/3] nano material centrifuge separation, and washed with dehydrated alcohol
It washs 3 times, is dried in a vacuum, and be saved in vacuum.
Product (β-Fe is determined using X-ray diffraction3Se4)4[Fe(TETA)4/3] crystal structure, crystal structure with
(β-Fe with tetragonal structure3Se4)4[Fe (TEPA)] is identical, as shown in Figure 7.As-deposited state Inorganic-Organic Hybrid Material
(β-Fe3Se4)4[Fe(TETA)4/3] nanometer sheet (a) 300K and low temperature (b) 5K hysteresis loop, as shown in Figure 8.
Embodiment 3
Ferric acetyl acetonade (4.375mmol), chromium acetylacetonate (0.875mmol) and selenium dioxide (6mmol) are dissolved in three
It in ethylene tetramine (TETA, 60ml), is placed in four-hole boiling flask, after leading to high pure nitrogen exclusion air, under magnetic stirring, will mix
Solution is warming up to 180 DEG C, keeps the temperature 0.5 hour；Mixed solution is warming up to 300 DEG C again, keeps the temperature 3 hours, it is miscellaneous to obtain inorganic-organic
Change nano material.It is cooled to room temperature, hybrid nano-material is centrifugated, and is washed 3 times with dehydrated alcohol, is done in a vacuum
It is dry, and be saved in vacuum.(β-Fe2.5Cr0.5Se4)4The X-ray diffraction figure of [Fe (TETA)], as shown in Figure 9.
Embodiment 4
By ferric acetyl acetonade (4.375mmol), chromium acetylacetonate (0.875mmol), selenium dioxide (3mmol) and antimony sodium
(3mmol) is dissolved in triethylene tetramine (TETA, 60ml), is placed in four-hole boiling flask, after leading to high pure nitrogen exclusion air, in magnetic
Under stirring, mixed solution is warming up to 180 DEG C, keeps the temperature 0.5 hour；Mixed solution is warming up to 300 DEG C again, 3 hours is kept the temperature, obtains
Obtain inorganic-organic hybridization (β-Fe2.5Cr0.5Se2Te2)4[Fe (TETA)] nano material.It is cooled to room temperature, by hybrid nano-material
Centrifuge separation, and washed 3 times with dehydrated alcohol, it is dried in a vacuum, and be saved in vacuum.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (10)
1. the orderly inorganic-organic hybrid functional nano-materials with room-temperature ferromagnetic, it is characterised in that: use chemical liquid phase legal system
Standby, the inorganic-organic hybrid functional nano-materials have two-dimensional nano piece or Nanoparticulate microstructure, inorganic structure unit
For the β-Fe with tetragonal structure3-xMxSe4-yQy, wherein M=Cr, Co；Q=S, Te；0≤x<3；0≤y < 4, organic structure
Unit is metal organo-amine complex.
2. according to the orderly inorganic-organic hybrid functional nano-materials described in claim 1 with room-temperature ferromagnetic, it is characterised in that:
The inorganic-organic hybrid functional nano-materials have the crystal structure of periodic arrangement.
3. according to the orderly inorganic-organic hybrid functional nano-materials described in claim 1 with room-temperature ferromagnetic, it is characterised in that:
The inorganic-organic hybrid functional nano-materials have the ferrimagnetism of room temperature.
4. according to the preparation method of the orderly inorganic-organic hybrid functional nano-materials described in claim 1 with room-temperature ferromagnetic,
It is characterized in that, is prepared using chemical liquid phase reaction, the specific steps are as follows:
(1) raw material are mixed with organic amine, is placed in 250 milliliters of -2000 milliliters of four-hole boiling flasks and is allowed to dissolve, before obtaining uniformly
Drive liquid solution；It is passed through inert gas and excludes air, under magnetic stirring, be warming up to 120-200 DEG C, keep the temperature 0-120 minutes；Again will before
It drives liquid solution and is warming up to reaction temperature, keep the temperature -24 hours 0.5 hour in the reaction temperature, after reaction, reaction system is dropped
To room temperature；
(2) it is centrifugated reaction product solution, supernatant is abandoned, obtains precipitated product；
(3) it after being washed with dehydrated alcohol, is dried in a vacuum, obtains powder product.
5. according to the preparation method of the orderly inorganic-organic hybrid functional nano-materials described in claim 4 with room-temperature ferromagnetic,
Be characterized in that: raw material described in step (1) include the metal precursor and selenium that are dissolvable in water organic amine, the forerunner of sulphur or tellurium
Body.
6. according to the preparation method of the orderly inorganic-organic hybrid functional nano-materials described in claim 5 with room-temperature ferromagnetic,
Be characterized in that: the metal precursor for being dissolvable in water organic amine is ferric acetyl acetonade, acetylacetone,2,4-pentanedione is ferrous, chromium acetylacetonate,
One or more mixing of acetylacetone cobalt, nickel acetylacetonate and manganese acetylacetonate；It is dissolvable in water the selenium of organic amine, sulphur or tellurium
Presoma is one of selenium powder, selenium dioxide, sodium selenide, vulcanized sodium, telluride sodium or a variety of.
7. according to the preparation method of the orderly inorganic-organic hybrid functional nano-materials described in claim 4 with room-temperature ferromagnetic,
Be characterized in that: the molar ratio of metallic atom and sulfur family atom is between 1:1 to 1:2 in the raw material.
8. according to the preparation method of the orderly inorganic-organic hybrid functional nano-materials described in claim 4 with room-temperature ferromagnetic,
Be characterized in that: organic amine solvent described in step (1) be diethylenetriamine, triethylene tetramine (triethylenetetramine,
TETA), in tetraethylenepentamine (tetraethylenepentamine, TEPA) and pentaethylene hexamine it is one or more.
9. according to the preparation method of the orderly inorganic-organic hybrid functional nano-materials described in claim 4 with room-temperature ferromagnetic,
Be characterized in that: raw material usage described in step (1) is 0.05-120 mMs, 20-1000 milliliters of organic solvent.
10. according to the preparation method of the orderly inorganic-organic hybrid functional nano-materials described in claim 4 with room-temperature ferromagnetic,
It is characterized by: reaction temperature described in step (1) is 180-300 DEG C.
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Cited By (2)
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| CN111850389A (en) * | 2019-04-29 | 2020-10-30 | 中国科学院金属研究所 | Method for preparing iron nitride nanorod material |
| CN115959634A (en) * | 2022-12-02 | 2023-04-14 | 中国科学院苏州纳米技术与纳米仿生研究所 | Carbon-coated NiSe 2 Composite nano material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111850389A (en) * | 2019-04-29 | 2020-10-30 | 中国科学院金属研究所 | Method for preparing iron nitride nanorod material |
| CN115959634A (en) * | 2022-12-02 | 2023-04-14 | 中国科学院苏州纳米技术与纳米仿生研究所 | Carbon-coated NiSe 2 Composite nano material and preparation method and application thereof |
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